3-(Trifluoromethyl)pyrrolidine → HCID 71285706, 화합물

HRID 536519노트

반응식

HRID 536519 반응식
[F:1][C:2]1[CH:30]=[CH:29][CH:28]=[CH:27][C:3]=1[CH2:4][N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[C:7]([C:14]2[N:15]=[C:16](I)[C:17]3[C:22]([CH3:24])([CH3:23])[C:21](=[O:25])[NH:20][C:18]=3[N:19]=2)=[N:6]1.[F:31][C:32]([F:39])([F:38])[CH:33]1[CH2:37][CH2:36][NH:35][CH2:34]1>CN1C(=O)CCC1>[F:1][C:2]1[CH:30]=[CH:29][CH:28]=[CH:27][C:3]=1[CH2:4][N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[C:7]([C:14]2[N:15]=[C:16]([N:35]3[CH2:36][CH2:37][CH:33]([C:32]([F:39])([F:38])[F:31])[CH2:34]3)[C:17]3[C:22]([CH3:24])([CH3:23])[C:21](=[O:25])[NH:20][C:18]=3[N:19]=2)=[N:6]1

참가 물질

4

반응물 2

HCID 51521593-(Trifluoromethyl)pyrrolidineHCID 86705367HCID 86705367, 화합물

생성물 1

HCID 71285706HCID 71285706, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
150 °C

실험 절차

Under an argon atmosphere, 200 mg (purity 62%, 0.24 mmol) of 2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4-iodo-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one (example 15A) was put in 4 ml of absolute NMP and 671 mg (4.82 mmol) of 3-(trifluoromethyl)pyrrolidine was added. The mixture was heated in the microwave at 150° C. for 5 h. The reaction solution was filtered and purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→100:0). 65 mg (49% of theor.) of the target compound was obtained.

후처리

  1. filtrationThe reaction solution was filtered
  2. custompurified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→100:0)
  3. custom65 mg (49% of theor.) of the target compound was obtained

출처 및 근거

ORD 기록
ord-1118da7cbd6149efb483f86ed714f2f3
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859569B2

반응 노트

불러오는 중…