HRID1721235

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6342

Acetonitrile

C2H3N

HCID521998

4-Methylbenzenesulfonic acid hydrate

C7H10O4S

结构：CC(C)(C)OC(=O)c1ccc(CC(N=C(c2ccccc2)c2ccccc2)C(=O)OCc2ccccc2)cc1

HCID14888672

未命名化合物

PRODUCTS

生成物

结构：CC(C)(C)OC(=O)c1ccc(CC(N)C(=O)OCc2ccccc2)cc1.Cc1ccc(S(=O)(=O)O)cc1

HCID86746526

未命名化合物

收率 68.2%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID962

Water

H2O

PROCEDURE

实验过程

A solution of rac.-2-[(diphenylmethylene)amino]-3-[4-[(1,1-dimethylethoxy)carbonyl]phenyl]propanoic acid benzyl ester (11.5 g, 22 mmol) and p-toluenesulfonic acid monohydrate (4.18 g, 22 mmol) in a 10/1 mixture of acetonitrile and water (640 ml) was stirred for 2 h at room temperature. Concentration provided a crude solid product which was recrystallized from ethanol-ether to give rac.-2-amino-3-[4-[(1,1-dimethylethoxy)carbonyl]phenyl]propanoic acid benzyl ester p-toluenesulfonic acid salt, (8.1 g, 15 mmol) in 67% yield, mp. 154°-157° C.

WORKUP

后处理

concentrationConcentration
customprovided a crude solid product which
customwas recrystallized from ethanol-ether

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-99f0e3a2e2224d04a494f9bda1b072f2
来源数据集: uspto-grants-1996_04
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05508437
来源说明: uspto-grants-1996_04

反应 SMILES

[CH2:1]([O:8][C:9](=[O:39])[CH:10]([N:25]=C(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH:14][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[C:41]1([CH3:51])[CH:46]=[CH:45][C:44]([S:47]([OH:50])(=[O:49])=[O:48])=[CH:43][CH:42]=1.C(#N)C>O>[C:41]1([CH3:51])[CH:42]=[CH:43][C:44]([S:47]([OH:50])(=[O:48])=[O:49])=[CH:45][CH:46]=1.[CH2:1]([O:8][C:9](=[O:39])[CH:10]([NH2:25])[CH2:11][C:12]1[CH:13]=[CH:14][C:15]([C:18]([O:20][C:21]([CH3:22])([CH3:24])[CH3:23])=[O:19])=[CH:16][CH:17]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1