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

Benzyl Alcohol → 8-(2-Benzyloxy-pyridine-3-sulfonyl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one

HRID 2194176
노트
인쇄 미리보기

반응식

HRID 2194176 반응식
[H-].[Na+].[CH2:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl[C:12]1[C:17]([S:18]([N:21]2[CH2:42][CH2:41][C:24]3([C:28](=[O:29])[N:27]([C:30]4[CH:35]=[CH:34][C:33]([O:36][C:37]([F:40])([F:39])[F:38])=[CH:32][CH:31]=4)[CH2:26][CH2:25]3)[CH2:23][CH2:22]2)(=[O:20])=[O:19])=[CH:16][CH:15]=[CH:14][N:13]=1>CN(C=O)C.C(OCC)(=O)C>[CH2:3]([O:10][C:12]1[C:17]([S:18]([N:21]2[CH2:22][CH2:23][C:24]3([C:28](=[O:29])[N:27]([C:30]4[CH:31]=[CH:32][C:33]([O:36][C:37]([F:38])([F:39])[F:40])=[CH:34][CH:35]=4)[CH2:26][CH2:25]3)[CH2:41][CH2:42]2)(=[O:20])=[O:19])=[CH:16][CH:15]=[CH:14][N:13]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 244Benzyl AlcoholHCID 24758Sodium hydrideHCID 595779608-(2-Chloro-pyridine-3-sulfonyl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one

생성물 1

HCID 667872738-(2-Benzyloxy-pyridine-3-sulfonyl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one수율 89%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
2회
HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

To a suspension of NaH (12 mg, 0.31 mmol) in DMF (2 mL) at 0° C. was added benzyl alcohol (25 uL, 0.25 mmol) and the mixture was stirred for 30 min at 0° C. A solution of 8-(2-chloro-pyridine-3-sulfonyl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one (described in example 188, 100 mg, 0.20 mmol) in DMF (500 uL) was added drop-wise and the reaction mixture was allowed to warm to room temperature and stirred for 16 h. The reaction mixture was diluted with ethyl acetate and washed with brine. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo to give the crude residue which was purified by flash column chromatography (1:2 AcOEt/heptane) which afforded the desired product as a colourless solid (100 mg, 87%). MS (ESI): 562.3 (MH+).

후처리

  1. temperatureto warm to room temperature
  2. stirringstirred for 16 h
  3. washwashed with brine
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto give the crude residue which
  8. customwas purified by flash column chromatography (1:2 AcOEt/heptane) which

출처 및 근거

ORD 기록
ord-d6f9e6e7b35847b49701834aca5fc2e4
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08329904B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트