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

Hydrochloric Acid → HCID 58579532, 화합물

HRID 1662211
노트
인쇄 미리보기

반응식

HRID 1662211 반응식
Br[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[CH:3]=1.C([Li])(C)(C)C.[Br:17][C:18]1[CH:19]=[C:20](/[C:26](/[C:34]2[CH:39]=[CH:38][CH:37]=[C:36]([F:40])[C:35]=2[C:41]#[N:42])=[N:27]\S(C(C)(C)C)=O)[CH:21]=[CH:22][C:23]=1[O:24][CH3:25].Cl.CO>C1COCC1>[Br:17][C:18]1[CH:19]=[C:20]([C:26]2([C:2]3[CH:7]=[CH:6][N:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[CH:3]=3)[C:34]3[C:35](=[C:36]([F:40])[CH:37]=[CH:38][CH:39]=3)[C:41]([NH2:42])=[N:27]2)[CH:21]=[CH:22][C:23]=1[O:24][CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 887MethanolHCID 234369504-Bromo-2-(trifluoromethyl)pyridineHCID 58579491(NE)-N-[(3-bromo-4-methoxyphenyl)-(2-cyano-3-fluorophenyl)methylidene]-2-methylpropane-2-sulfinamideHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 58579532HCID 58579532, 화합물
수율 89.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

A solution of 4-bromo-2-trifluoromethylpyridine (1.76 g, 7.80 mmol) in THF (2 mL) was added dropwise at −100° C. to t-butyllithium (9.17 mL, 15.59 mmol) in THF (15 mL) followed by the addition of (E)-N-((3-bromo-4-methoxyphenyl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide (3.1 g, 7.09 mmol) in THF (10 mL). The reaction mixture was left on a thawing cooling bath for 1 hour and then allowed to reach room temperature and stirred for 2.5 hours. Hydrochloric acid in methanol (1.25 M, 28.4 mL, 35.4 mmol) was added and the reaction was stirred for 1 hour. Silica powder was added and the mixture was concentrated under reduced pressure. The residue was purified by flash column chromatography (0-10% 0.1M NH3 in methanol in DCM) to afford the title compound (3.04 g, 89%).

후처리

  1. waitThe reaction mixture was left on a thawing
  2. temperaturecooling bath for 1 hour
  3. customto reach room temperature
  4. stirringthe reaction was stirred for 1 hour
  5. additionSilica powder was added
  6. concentrationthe mixture was concentrated under reduced pressure
  7. customThe residue was purified by flash column chromatography (0-10% 0.1M NH3 in methanol in DCM)

출처 및 근거

ORD 기록
ord-a095c90993e64ef8a02dec7dd0dbca61
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030500B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트