Water → HCID 68294330、化合物

HRID 2279482ノート

反応式

HRID 2279482 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]([NH2:14])[C:10]([F:13])([F:12])[F:11])[CH:5]=[CH:6][C:7]=1[Cl:8].[C:15](Cl)(=[O:26])[O:16][C:17]1[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=1.N1C=CC=CC=1.O>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]([NH:14][C:15](=[O:26])[O:16][C:17]2[CH:18]=[CH:19][C:20]([N+:23]([O-:25])=[O:24])=[CH:21][CH:22]=2)[C:10]([F:11])([F:12])[F:13])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 821294-Nitrophenyl chloroformateHCID 433445253,4-Dichloro-α-(trifluoromethyl)benzenemethanamine

生成物 1

HCID 68294330HCID 68294330、化合物収率 92.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 148 (1.00 g, 4.01 mmol), 4-nitrophenyl carbonochloridate (0.9085 g, 4.507 mmol) and pyridine (0.7131 g, 9.015 mmol) in DCM (10 mL) were stirred for 30 min. Water was added and the reaction mixture was extracted with DCM. The organic layer was concentrated and purified by SiO2 chromatography eluting with 20% EtOAc/hexane to afford 1.511 g (90.0%) of 4-nitrophenyl 1-(3,4-dichlorophenyl)-2,2,2-trifluoroethylcarbamate (150).

後処理

  1. extractionthe reaction mixture was extracted with DCM
  2. concentrationThe organic layer was concentrated
  3. custompurified by SiO2 chromatography
  4. washeluting with 20% EtOAc/hexane

出典と根拠

ORDレコード
ord-6a73b7652f5444e690bb4d495dfcc7ea
出典データセット
uspto-grants-2015_09
特許番号
US09133187B2

反応ノート

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