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

Diisopropylethylamine → (S)-9-Fluoro-5-[3-phenethyl-piperazine-1-yl]-11H-12-thia-6,11-diaza-dibenzo[a,f]azulene

HRID 1350486
노트
인쇄 미리보기

반응식

HRID 1350486 반응식
Cl.[F:2][C:3]1[CH:4]=[CH:5][C:6]2[N:15]=[C:14]([NH2:16])[C:13]3[C:12]4[CH:17]=[CH:18][CH:19]=[CH:20][C:11]=4[S:10][C:9]=3[NH:8][C:7]=2[CH:21]=1.[CH2:22]([C@H:30]1[CH2:35]N[CH2:33][CH2:32][NH:31]1)[CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(N(C(C)C)CC)(C)C>CS(C)=O.C1(C)C=CC=CC=1.C(Cl)Cl>[F:2][C:3]1[CH:4]=[CH:5][C:6]2[N:15]=[C:14]([N:16]3[CH2:33][CH2:32][NH:31][C@@H:30]([CH2:22][CH2:23][C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=4)[CH2:35]3)[C:13]3[C:12]4[CH:17]=[CH:18][CH:19]=[CH:20][C:11]=4[S:10][C:9]=3[NH:8][C:7]=2[CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 81531DiisopropylethylamineHCID 1842238412-Amino-8-fluoro-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine hydrochlorideHCID 44828673(S)-2-Phenethylpiperazine

생성물 1

HCID 24887774(S)-9-Fluoro-5-[3-phenethyl-piperazine-1-yl]-11H-12-thia-6,11-diaza-dibenzo[a,f]azulene수율 33.3%

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide
용매
HCID 1140Toluene용매
HCID 6344Dichloromethane용매

반응 조건

온도
115 °C

실험 절차

Combine 9-fluoro-11H-12-thia-6,11-diaza-dibenzo[a,f]azulen-5-ylamine hydrogen chloride (287 mg, 0.9 mmol), (S)-2-phenethyl-piperazine (340 mg, 1.80 mmol) and diisopropylethyl amine (116 mg, 0.9 mmol) in DMSO (0.5 mL) and toluene (2.0 mL), stir and microwave (300 W, 125 ° C.) for 8 h, then heat to 115 ° C. for 22 h. Cool the reaction to RT, dilute with CH2Cl2, wash with H2O and brine. Dry the organic layer with by Na2SO4. The crude material purify by chromatography on silica gel, gradient (100% CH2Cl2 to 100% CH2Cl2:2N NH3/MeOH=25:1), give 137 mg of title compound.

후처리

  1. temperatureCool
  2. customthe reaction to RT
  3. washwash with H2O and brine
  4. dry with materialDry the organic layer with by Na2SO4
  5. customThe crude material purify by chromatography on silica gel, gradient (100% CH2Cl2 to 100% CH2Cl2:2N NH3/MeOH=25:1)

출처 및 근거

ORD 기록
ord-8d1e6ef4da8247849abf56d6c85f1e8f
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214673B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트