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

Dichloromethane → HCID 22182461, 화합물

HRID 1796810
노트
인쇄 미리보기

반응식

HRID 1796810 반응식
ClCCl.[CH3:4][NH:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]3[CH:30]=[C:29]([F:31])[CH:28]=[CH:27][C:26]=3[CH3:32])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[CH:10]([C:33]23OCC(C)(C[O:38]2)C[O:34]3)[CH:9]1[CH3:42])=[O:7].FC(F)(F)C(O)=O>O>[F:31][C:29]1[CH:28]=[CH:27][C:26]([CH3:32])=[C:25]([CH:30]=1)[CH2:24][O:23][C:20]1[CH:19]=[CH:18][C:17]([S:14]([N:11]2[CH2:12][CH2:13][N:8]([C:6](=[O:7])[NH:5][CH3:4])[CH:9]([CH3:42])[CH:10]2[C:33]([OH:38])=[O:34])(=[O:16])=[O:15])=[CH:22][CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 69597599HCID 69597599, 화합물

생성물 1

HCID 22182461HCID 22182461, 화합물수율 102.7%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

To a dichloromethane (7 ml) solution of 4-[4-(5-fluoro-2-methyl-benzyloxy)-benzenesulfonyl]-2-methyl-3-(4-methyl-2,6,7-trioxa-bicyclo[2.2.2]oct-1-yl)-piperazine-1-carboxylic acid methylamide (compound of formula XLIV, 376 mg, 0.67 mmol) at about 23° C. was added water (0.14 ml) and trifluoroacetic acid (0.14 ml). The reaction mixture was stirred for about 0.5 hour then was concentrated in vacuo. The residue was diluted with methanol (20 ml) and water (6 ml) and cesium carbonate (45 ml of a 10% solution in water) was added to the mixture. The reaction mixture was heated to about 40° C. for about 24 hours then was cooled to about 23° C., acidified with hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with brine and dried with sodium sulfate and concentrated in vacuo, to give 330 mg of a compound of formula XLVI.

후처리

  1. concentrationthen was concentrated in vacuo
  2. additionThe residue was diluted with methanol (20 ml) and water (6 ml) and cesium carbonate (45 ml of a 10% solution in water)
  3. additionwas added to the mixture
  4. temperaturethen was cooled to about 23° C.
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with brine
  7. dry with materialdried with sodium sulfate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c33980ed2ba74a3cafe5ed8fb8bef2eb
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030242B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트