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

Acetic Acid → 7-chloro-1-methyl-1H-pyrrolo[2,3-c]pyridine

HRID 1711037
노트
인쇄 미리보기

반응식

HRID 1711037 반응식
[Cl:1][C:2]1[N:3]=[CH:4][CH:5]=[C:6]2[CH:10]=[CH:9][NH:8][C:7]=12.[H-].[Na+].CI.[C:15](O)(=O)C>CN(C=O)C>[Cl:1][C:2]1[N:3]=[CH:4][CH:5]=[C:6]2[CH:10]=[CH:9][N:8]([CH3:15])[C:7]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 114350487-Chloro-1H-pyrrolo[2,3-c]pyridine

생성물 1

HCID 594244767-chloro-1-methyl-1H-pyrrolo[2,3-c]pyridine수율 92%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

실험 절차

To a solution of 259 (250 mg, 1.64 mmol) in DMF (16 mL) at 0° C. was added NaH (197 mg, 4.92 mmol, 60% in mineral oil), and the mixture was stirred for 30 min, followed by addition of MeI (112 □L, 1.80 mmol). The reaction mixture was stirred at room temperature for 2 h before acetic acid (1 mL) was added. Solvents were removed under reduced pressure, the residue was partitioned between water and EtOAc. Organic phase was collected, dried over anhydrous Na2SO4 and concentrated. The residue was purified by flash column chromatography, eluent EtOAc/hexane (1:1), to afford the title compound 263 (200 mg, 92% yield) as an off-white solid. MS (m/z): 167.1 (M+H) (found).

후처리

  1. additionwas added
  2. customSolvents were removed under reduced pressure
  3. customthe residue was partitioned between water and EtOAc
  4. customOrganic phase was collected
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated
  7. customThe residue was purified by flash column chromatography, eluent EtOAc/hexane (1:1)

출처 및 근거

ORD 기록
ord-865abc7761884e8dbd96128d27840337
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790729B2

반응 노트

불러오는 중…