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

Water → (2RS)-2-(7-chloro-2-cyano-10-phenothiazinyl)propyl methanesulphonate

HRID 704225
노트
인쇄 미리보기

반응식

HRID 704225 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[CH:10]=[C:11]2[C:20](=[CH:21][CH:22]=1)[N:19]([CH:23]([CH3:26])[CH2:24][OH:25])[C:18]1[CH:17]=[C:16]([C:27]#[N:28])[CH:15]=[CH:14][C:13]=1[S:12]2.[CH3:29][S:30](Cl)(=[O:32])=[O:31].O>C(Cl)Cl>[CH3:29][S:30]([O:25][CH2:24][CH:23]([N:19]1[C:18]2[CH:17]=[C:16]([C:27]#[N:28])[CH:15]=[CH:14][C:13]=2[S:12][C:11]2[C:20]1=[CH:21][CH:22]=[C:9]([Cl:8])[CH:10]=2)[CH3:26])(=[O:32])=[O:31]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 159253677-chloro-10-[(2RS)-1-hydroxy-2-propyl]-2-phenothiazinecarbonitrile

생성물 1

HCID 15925250(2RS)-2-(7-chloro-2-cyano-10-phenothiazinyl)propyl methanesulphonate

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

반응 조건

온도
0 °C

실험 절차

Triethylamine (30 cc) is added to a solution of 7-chloro-10-[(2RS)-1-hydroxy-2-propyl]-2-phenothiazinecarbonitrile (40 g) in methylene chloride (400 cc). The mixture is cooled to 0° C. and then treated dropwise in the course of 1 hour with methanesulphonyl chloride (16.6 cc). Distilled water (1 liter) is then added, after which the constituents of the mixture are allowed to settle and the organic phase is separated and washed with distilled water (500 cc). The organic phase is then dried over magnesium sulphate, filtered and concentrated under reduced pressure (30 mm Hg; 4 kPa) to a residual volume of 100 cc. Isopropyl ether (150 cc) is then introduced slowly and the mixture is left stirred for 30 minutes. Isopropyl ether (300 cc) is then added slowly and the suspension is stirred for 48 hours. The precipitate is filtered off, washed with isopropyl ether (2×50 cc) and dried at 40° C. under reduced pressure (5 mm Hg; 0.67 kPa) to give (2RS)-2-(7-chloro-2-cyano-10-phenothiazinyl)propyl methanesulphonate (34.53 g), m.p. 132° C.

후처리

  1. customthe organic phase is separated
  2. washwashed with distilled water (500 cc)
  3. dry with materialThe organic phase is then dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure (30 mm Hg; 4 kPa) to a residual volume of 100 cc
  6. additionIsopropyl ether (150 cc) is then introduced slowly
  7. waitthe mixture is left
  8. additionIsopropyl ether (300 cc) is then added slowly
  9. stirringthe suspension is stirred for 48 hours
  10. filtrationThe precipitate is filtered off
  11. washwashed with isopropyl ether (2×50 cc)
  12. customdried at 40° C. under reduced pressure (5 mm Hg; 0.67 kPa)

출처 및 근거

ORD 기록
ord-86e05c2815c14a46aec0bf94ede06c9e
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04985419

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트