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

Tetrahydrofuran → 4-[2-Cyano-3-[[(3s)-hexahydro-2-oxo-1-[2-oxo-2-(1-pyrrolidinyl)ethyl]-1h-azepin-3-yl]amino]-3-[(2-methyl-5-benzofuranyl)amino]-1-oxo-2-propenyl]benzoic acid

HRID 1264628
노트
인쇄 미리보기

반응식

HRID 1264628 반응식
C[O:2][C:3](=[O:44])[C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:43])[C:11]([C:41]#[N:42])=[C:12]([NH:24][C@H:25]2[CH2:31][CH2:30][CH2:29][CH2:28][N:27]([CH2:32][C:33](=[O:39])[N:34]3[CH2:38][CH2:37][CH2:36][CH2:35]3)[C:26]2=[O:40])[NH:13][C:14]2[CH:15]=[CH:16][C:17]3[O:21][C:20]([CH3:22])=[CH:19][C:18]=3[CH:23]=2)=[CH:6][CH:5]=1.C1COCC1>O>[C:41]([C:11](=[C:12]([NH:24][C@H:25]1[CH2:31][CH2:30][CH2:29][CH2:28][N:27]([CH2:32][C:33](=[O:39])[N:34]2[CH2:35][CH2:36][CH2:37][CH2:38]2)[C:26]1=[O:40])[NH:13][C:14]1[CH:15]=[CH:16][C:17]2[O:21][C:20]([CH3:22])=[CH:19][C:18]=2[CH:23]=1)[C:10]([C:7]1[CH:8]=[CH:9][C:4]([C:3]([OH:44])=[O:2])=[CH:5][CH:6]=1)=[O:43])#[N:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8028TetrahydrofuranHCID 700328734-[2-Cyano-3-[[(3S)-hexahydro-2-oxo-1-[2-oxo-2-(1-pyrrolidinyl)ethyl]-1H-azepin-3-yl]amino]-3-[(2-methyl-5-benzofuranyl)amino]-1-oxo-2-propenyl]benzoic acid methyl ester

생성물 1

HCID 700323634-[2-Cyano-3-[[(3s)-hexahydro-2-oxo-1-[2-oxo-2-(1-pyrrolidinyl)ethyl]-1h-azepin-3-yl]amino]-3-[(2-methyl-5-benzofuranyl)amino]-1-oxo-2-propenyl]benzoic acid수율 83.4%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

The compound of Example 1 (0.442g, 0.740 mmol) was dissolved in 10 mL of 1:1 water:THF and the mixture was cooled to 0° C. To the solution was added LiOH monohydrate (0.31 g, 7.4 mmol). The reaction mixture was allowed to come to room temperature. After stirring for 24 h, the reaction mixture was concentrated by in vacuo and the residue was dissolved in methylene chloride. The mixture was extracted 2×25 mL with water. The combined aqueous layers were neutralized with 1 N HCl to pH 4 and were extracted 2×25 mL with ethyl acetate. The combined ethyl acetate layers were dried over sodium sulfate and concentrated to give the title compound (360 mg, 83%) as yellow solid: MS (ESI, pos. ion) m/z 584 (M+H); HPLC (method B) tR=3.8 min, purity: >96%.

후처리

  1. customto come to room temperature
  2. concentrationthe reaction mixture was concentrated by in vacuo
  3. dissolutionthe residue was dissolved in methylene chloride
  4. extractionThe mixture was extracted 2×25 mL with water
  5. extractionwere extracted 2×25 mL with ethyl acetate
  6. dry with materialThe combined ethyl acetate layers were dried over sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2e86c2a03dc3463cb6dabee706c20811
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06544981B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트