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

Thionyl Chloride → 3-Chloromethyl-5,6-dimethoxy-1-(1-trityl-4-imidazolyl)methyl-1H-indazole

HRID 617630
노트
인쇄 미리보기

반응식

HRID 617630 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[N:8]([CH2:14][C:15]1[N:16]=[CH:17][N:18]([C:20]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:19]=1)[N:7]=[C:6]2[CH2:39]O.S(Cl)([Cl:43])=O.C(Cl)(Cl)Cl.C(O)C.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:43][CH2:39][C:6]1[C:5]2[C:9](=[CH:10][C:11]([O:12][CH3:13])=[C:3]([O:2][CH3:1])[CH:4]=2)[N:8]([CH2:14][C:15]2[N:16]=[CH:17][N:18]([C:20]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:19]=2)[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 154286385,6-dimethoxy-1-(1-trityl-4-imidazolyl)methyl-1H-indazole-3-methanolHCID 21889567Chloroform ethanol

생성물 1

HCID 154286393-Chloromethyl-5,6-dimethoxy-1-(1-trityl-4-imidazolyl)methyl-1H-indazole

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

5,6-Dimethoxy-1-(1-trityl-4-imidazolyl)methyl-1H-indazole-3-methanol (180.0 g) was ground into a powder form using a mortar and suspended in dichloromethane (1,700 ml) at room temperature. After suspension, the reaction solution was stirred with cooling in an ice bath. To this was added dropwise 48.6 ml of thionyl chloride spending 5 minutes. It was observed 1 minute thereafter that the spot of the material almost disappeared on a thin layer chromatography (chloroform/ethanol=30/1). The reaction solution was poured into saturated sodium bicarbonate aqueous solution (2,000 ml) and extracted with chloroform (5,000 ml), and the extract was dried with sodium sulfate, filtered and then evaporated under a reduced pressure to obtain colorless solid (165.1 g). This solid substance was used in the subsequent reaction as such.

후처리

  1. temperaturewith cooling in an ice bath
  2. extractionextracted with chloroform (5,000 ml)
  3. dry with materialthe extract was dried with sodium sulfate
  4. filtrationfiltered
  5. customevaporated under a reduced pressure

출처 및 근거

ORD 기록
ord-01fda1a5764a4ddc9b03174ac6869a51
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05948913

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트