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

Sodium Methoxide → Trans-2-methyl-7-(trifluoromethoxy)-1,2,3,3a,4,5-hexahydrobenzo[c]pyrrolo[3,4-e]azepin-6(10bH)-one

HRID 84948
노트
인쇄 미리보기

반응식

HRID 84948 반응식
[NH2:1][CH2:2][C@H:3]1[CH2:7][N:6]([CH3:8])[CH2:5][C@@H:4]1[C:9]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[C:10]=1[C:11](OC)=[O:12].C[O-].[Na+]>CO>[CH3:8][N:6]1[CH2:7][C@@H:3]2[C@H:4]([C:9]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[C:10]=3[C:11](=[O:12])[NH:1][CH2:2]2)[CH2:5]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 67168219Methyl 2-((3S,4S)-4-(aminomethyl)-1-methylpyrrolidin-3-yl)-6-(trifluoromethoxy)benzoate

생성물 1

HCID 54673517Trans-2-methyl-7-(trifluoromethoxy)-1,2,3,3a,4,5-hexahydrobenzo[c]pyrrolo[3,4-e]azepin-6(10bH)-one

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
70 °C

실험 절차

The product obtained from Example 110B (5.5 g) was dissolved in 25 mL of methanol and treated with 5 mL of 25 weight % sodium methoxide in methanol. The reaction was stirred and heated at 70° C. for 16 hours. The reaction was cooled and concentrated, and the residue was purified via flash chromatography on a silica gel column (95:5 dichloromethane:2 N ammonia in methanol) to afford the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 2.04-2.20 (m, 1H) 2.41 (s, 3H) 2.62 (dd, J=10.85 Hz, 8.82 Hz, 1H) 2.73 (t, J=8.31 Hz, 1H) 2.93-3.01 (m, 3H) 3.03-3.14 (m, 2H) 7.24 (d, J=7.80 Hz, 1H) 7.32 (d, J=8.14 Hz, 1H) 7.51-7.59 (m, 1H) 8.33 (t, J=5.76 Hz, 1H); MS (DCI+) m/z 301.1 [M+H]+.

후처리

  1. temperatureThe reaction was cooled
  2. concentrationconcentrated
  3. customthe residue was purified via flash chromatography on a silica gel column (95:5 dichloromethane:2 N ammonia in methanol)

출처 및 근거

ORD 기록
ord-f3c654f78d904ef9b111f3be614c5ddb
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846951B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트