Water → HCID 68294330, 화합물

HRID 2279482노트

반응식

HRID 2279482 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 68294330HCID 68294330, 화합물수율 92.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6a73b7652f5444e690bb4d495dfcc7ea
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133187B2

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