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

Triphenylphosphine → {1-[4-(pentafluoro-lambda6-sulfanyl)phenyl]-1H-tetrazol-5-yl}methyl acetate

HRID 517729
노트
인쇄 미리보기

반응식

HRID 517729 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:20]([O:23][CH2:24][C:25](=O)[NH:26][C:27]1[CH:32]=[CH:31][C:30]([S:33]([F:38])([F:37])([F:36])([F:35])[F:34])=[CH:29][CH:28]=1)(=[O:22])[CH3:21].C[Si]([N:44]=[N+:45]=[N-:46])(C)C>C1COCC1.CCOC(C)=O>[C:20]([O:23][CH2:24][C:25]1[N:26]([C:27]2[CH:32]=[CH:31][C:30]([S:33]([F:38])([F:37])([F:36])([F:35])[F:34])=[CH:29][CH:28]=2)[N:46]=[N:45][N:44]=1)(=[O:22])[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11776TriphenylphosphineHCID 78378AzidotrimethylsilaneHCID 866918762-Oxo-2-{[4-(pentafluoro-lambda6-sulfanyl)phenyl]amino}ethyl acetate2회

생성물 1

HCID 86691878{1-[4-(pentafluoro-lambda6-sulfanyl)phenyl]-1H-tetrazol-5-yl}methyl acetate수율 59%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

Triphenylphosphine (16.2 g, 61.9 mmol) and diisopropylazodicorboxylate (12.5 g, 61.8 mmol) were added to a solution of 2-oxo-2-{[4-(pentafluoro-λ6-sulfanyl)phenyl]amino}ethyl acetate (Intermediate 42, 8.50 g, 26.2 mmol) in THF (100 mL) at 0° C. and the mixture was stirred for 30 min. Trimethylsilyl azide (7.11 g, 61.7 mmol) was added dropwise at room temperature and the mixture was heated to reflux for 4 hr. The reaction mixture was diluted with EtOAc and washed with ice-water and brine solution, dried over anhydrous Na2SO4, and concentrated under reduced pressure to give the crude product (5.32 g). This was used for the next step without further purification.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 4 hr
  3. washwashed with ice-water and brine solution
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1529a46bd46a40998a8e12d2b64ce543
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115132B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트