870822-87-0|tert-Butyl 2-(1-(4-(Ethoxycarbonyl)phenyl)ethylidenE)hydrazinecarboxylate| Ambeed

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CAS No. :	870822-87-0
Formula :	C₁₅H₂₀N₂O₄
M.W :	292.34
SMILES Code :	O=C(OC(C)(C)C)N/N=C(C)\C1=CC=C(C=C1)C(OC)=O
MDL No. :	N/A

Yield	Reaction Conditions	Operation in experiment
68.3%	With acetic acid; In toluene; at 80℃;	A solution of tert-butyl carbazate (14.0 g, 106.1 mmol) andcompound 2 (13.6 g, 70.8 mmol) in toluene (120 mL) with catalyticHOAc was stirred at 80 C overnight. tert-Butyl-2-{1-[4-(ethoxycarbonyl)phenyl]-ethylidene}hydrazine carboxylate was collectedby filtration as a crystalline solid (14.8 g, 68.3%). Without furtherpurification, NaBH3CN (3.3 g, 53.1 mmol) and tert-butyl 2-{1-[4-(ethoxycarbonyl)phenyl]ethylidene}-hydrazinecarboxylate (14.8g, 48.3 mmol) were dissolved in THF (120 mL). A solution of ptoluenesulfonicacid (9.7 g, 56.5 mmol) in THF (50 mL) was slowlyadded for 3 h and the reaction was detected by TLC. The mixturewas extracted with EtOAc and washed with brine, dried over anhydrousNa2SO4 and concentrated to give a white solid. The solid wasredissolved in DCM and washed with 1 N NaOH and the organiclayer was washed with 1 N HCl and brine, dried over Na2SO4 andconcentrated to yield white solid. Flash column chromatographypetroleum ether/ethyl acetate = 4/1 to yield 13.6 g (91%) tert-butyl2-{1-[4-(ethoxycarbonyl)-phenyl]ethyl}hydrazine carboxylate. 1HNMR (400 MHz, DMSO-d6) d 8.17 (s, 1H), 7.89 (d, J = 8.3 Hz, 2H),7.47 (d, J = 8.2 Hz, 2H), 4.73 (s, 1H), 4.30 (q, J = 7.1 Hz, 2H), 4.17(s, 1H), 1.33 (d, J = 6.2 Hz, 9H), 1.30 (d, J = 7.1 Hz, 3H), 1.18 (d, J =6.6 Hz, 3H). MS (ESI, m/z): 307.1 [MH].
65.7%	With acetic acid; In toluene; at 80℃;	A solution of tert-butyl carbazate(5.5 g, 41.6 mmol) and ethyl 4-acetylbenzoate (10 g, 52.0 mmol) intoluene (60 mL) with catalytic HOAc was stirred at 80 C overnight.tert-Butyl-2-{1-[4-(ethoxycarbonyl)phenyl]-ethylidene}hydrazinecarboxylate separated as a crystalline solid (10 g, 65.7%) and wascollected by filtration. NaBH3CN (2.4 g, 38.2 mmol) and tert-butyl2-{1-[4-(ethoxycarbonyl)phenyl]ethylidene}-hydrazinecarboxylate(10 g, 32.6 mmol) were dissolved in THF (100 mL). A solutionof p-toluene sulfonic acid (4.3 g, 22.6 mmol) in THF (25 mL) wasslowly added. After stirring the reaction for 3 h, the mixture wasextracted with EtOAc and washed with brine, dried (Na2SO4), andconcentrated to give a white solid. The solid was separated andwashed with 1 N HCl twice and brine twice, dried (Na2SO4), andconcentrated. Product precipitated as white solid and was washedwith petroleum ether/ethyl acetate (4:1) to yield 5.6 g (55.6%) oftert-butyl 2-{1-[4-(ethoxycarbonyl)-phenyl]ethyl}hydrazine carboxylate.1H NMR (400 MHz, CDCl3) d 8.01 (d, J = 8.3 Hz, 2H),7.41 (d, J = 8.3 Hz, 2H), 4.37 (q, J = 7.1 Hz, 2H), 4.22 (d, J = 6.4 Hz,1H), 1.41 (d, J = 2.7 Hz, 9H), 1.38 (d, J = 7.1 Hz, 3H), 1.35 (d,J = 6.6 Hz, 3H). MS (ESI, m/z): 307.1 [MH].
	In toluene; at 80℃; for 15h;	A solution of tert-butyl carbazate (13.90 g, 105 mmol) and ethyl 4-acetylbenzoate (20.00 g, 0.104 mol) in toluene (120 mL) was stirred at 80 C. overnight (15 h). tert-butyl-2-{1-[4-(ethoxycarbonyl)phenyl]ethylidene}hydrazinecarboxylate separated as crystalline solid and was collected by filtration of the mixture. HPLC/MS: m/z=307.3 (M+1)+, Rt=3.47 min. 1H NMR (500 MHz, CDCl3): delta 8.05 (2H, d, J=8.5 Hz), 7.88 (2H, d, J=8.5 Hz), 7.79 (1H, br s), 4.41 (2H, q, J=7.0 Hz), 2.24 (3H, s), 1.58 (9H, s), 1.43 (3H, t, J=7.0 Hz).

	In toluene; at 80℃; for 15h;	A solution of tert-butyl carbazate (13.90 g, 105 mmol) and ethyl 4-acetylbenzoate (20.00 g, 0.104 mol) in toluene (120 mL) was stirred at 80 0C overnight (15 h). tert-butyl-2-{ l-[4- (ethoxycarbonyl)phenyl]ethylidene}hydrazinecarboxylate separated as crystalline solid and was collected by filtration of the mixture. HPLC/MS: m/z = 307.3 (M+l)+, R1 = 3.47 min. 1H NMR (500 MHz, CDCl3): delta 8.05 (2H, d, J = 8.5 Hz), 7.88 (2H, d, J = 8.5 Hz), 7.79 (IH, br s), 4.41 (2H, q, J = 7.0 Hz), 2.24 (3H, s), 1.58 (9H, s), 1.43 (3H, t, J = 7.0 Hz).
	In toluene; at 80℃; for 15h;	Step A tert-Butyl 2-{1-[4-(ethoxycarbonyl)phenyl]ethylidene}hydrazinecarboxylate.; A solution of tert-butyl carbazate (13.90 g, 105 mmol) and ethyl 4-acetylbenzoate (20.00 g, 104 mmol) in toluene (120 mL) was stirred at 80 C. overnight (15 h). The title compound separated as crystalline solid and was collected by filtration of the mixture. HPLC/MS: m/z=307.3 (M+1)+, Rt=3.47 min. 1H NMR (500 MHz, CDCl3): delta 8.05 (d, J=8.5 Hz, 2H), 7.88 (d, J=8.5 Hz, 2H), 7.79 (br s, 1H), 4.41 (q, J=7.0 Hz, 2H), 2.24 (s, 3H), 1.58 (s, 9H), 1.43 (t, J=7.0 Hz, 3H).

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CAS No.: 870822-87-0

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CAS No.: 870822-87-0

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