HRID606762

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6214

Hexachloroethane

C2Cl6

HCID11776

Triphenylphosphine

C18H15P

HCID81531

Diisopropylethylamine

C8H19N

结构：CC(C)(C)OC(=O)N1CCC(=C(C(=O)NNC(=O)C2CN(C(=O)OCC3c4ccccc4-c4ccccc43)C2)c2ccccc2)CC1

HCID67046462

未命名化合物

PRODUCTS

生成物

结构：CC(C)(C)OC(=O)N1CCC(=C(c2ccccc2)c2nnc(C3CN(C(=O)OCC4c5ccccc5-c5ccccc54)C3)o2)CC1

HCID67046374

未命名化合物

收率 75%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

To a solution of 4-[1-phenyl-1-(2-(N-(9-fluorenylmethoxycarbonyl)-3-azetidinecarbonyl)-hydrazinocarbonyl)-methylene]-piperidine-1-carboxylic acid tert-butyl ester (0.411 g, 0.645 mmol), iPr2NEt (0.775 mL, 4.448 mmol) and PPh3 (0.693 g, 2.643 mmol) in CH3CN (8 mL) was added hexachloroethane (0.351 mg, 1.483 mmol). The mixture was allowed to stir for 1 h and then it was worked up as in Method A above and the crude product purified by flash chromatography (SiO2/EtOAc-hexane, 1:1) to give the title compound (0.299 g, 75%) as a colorless solid:

WORKUP

后处理

customthe crude product purified by flash chromatography (SiO2/EtOAc-hexane, 1:1)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-c3b1da05eaa74ca286516ffb967124ad
来源数据集: uspto-grants-2011_03
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07915283B2
来源说明: uspto-grants-2011_03

反应 SMILES

[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11](=[C:14]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)[C:15]([NH:17][NH:18][C:19]([CH:21]2[CH2:24][N:23]([C:25]([O:27][CH2:28][CH:29]3[C:41]4[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=4[C:35]4[C:30]3=[CH:31][CH:32]=[CH:33][CH:34]=4)=[O:26])[CH2:22]2)=[O:20])=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.ClC(Cl)(Cl)C(Cl)(Cl)Cl>CC#N>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][C:11](=[C:14]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)[C:15]2[O:20][C:19]([CH:21]3[CH2:22][N:23]([C:25]([O:27][CH2:28][CH:29]4[C:41]5[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=5[C:35]5[C:30]4=[CH:31][CH:32]=[CH:33][CH:34]=5)=[O:26])[CH2:24]3)=[N:18][N:17]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]