홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methyl iodide → (6'-Chloro-2-methyl-[3,4']bipyridinyl-3'-yl)-methyl-carbamic acid tert-butyl ester

HRID 347689
노트
인쇄 미리보기

반응식

HRID 347689 반응식
[C:1]([O:5][C:6](=[O:22])[NH:7][C:8]1[CH:9]=[N:10][C:11]([Cl:21])=[CH:12][C:13]=1[C:14]1[C:15]([CH3:20])=[N:16][CH:17]=[CH:18][CH:19]=1)([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[CH3:25]I>CN(C=O)C>[C:1]([O:5][C:6](=[O:22])[N:7]([C:8]1[CH:9]=[N:10][C:11]([Cl:21])=[CH:12][C:13]=1[C:14]1[C:15]([CH3:20])=[N:16][CH:17]=[CH:18][CH:19]=1)[CH3:25])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 58694598(6'-Chloro-2-methyl-[3,4']bipyridinyl-3'-yl)-carbamic acid tert-butyl ester

생성물 1

HCID 58694607(6'-Chloro-2-methyl-[3,4']bipyridinyl-3'-yl)-methyl-carbamic acid tert-butyl ester수율 84%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 0.16 g (0.50 mmol) (6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-yl)-carbamic acid tert-butyl ester in 5 ml DMF were added 25 mg (0.50 mmol) sodium hydride (50% suspension in mineral oil) under nitrogen at room temperature. After stirring for 30 min 0.034 ml (0.52 mmol) methyl iodide were added. The reaction mixture was stirred for 1 h. Quenching with water was followed by extraction with three portions of dichloromethane. The combined organic layers were washed with water. The combined aqueous layers were extracted with dichloromethane. The combined organic layers were dried with sodium sulfate and concentrated. Residual DMF was removed by Kugelrohr distillation. Flash chromatography gave 0.14 g (84%) of the title compound.

후처리

  1. additionwere added
  2. customQuenching with water
  3. extractionwas followed by extraction with three portions of dichloromethane
  4. washThe combined organic layers were washed with water
  5. extractionThe combined aqueous layers were extracted with dichloromethane
  6. dry with materialThe combined organic layers were dried with sodium sulfate
  7. concentrationconcentrated
  8. customResidual DMF was removed by Kugelrohr distillation

출처 및 근거

ORD 기록
ord-3477e95c22354478ba25ebd5b4ea1254
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07176205B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트