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Ammonia → 2-Amino-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one

HRID 925561
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인쇄 미리보기

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HRID 925561 반응식
Cl[C:2]1[N:3]([CH2:28][CH2:29][CH3:30])[C:4](=[O:27])[C:5]2[NH:6][C:7]([C:11]3[CH:12]=[N:13][N:14]([CH2:16][C:17]4[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=4)[CH:15]=3)=[N:8][C:9]=2[N:10]=1.[NH3:31]>>[NH2:31][C:2]1[N:3]([CH2:28][CH2:29][CH3:30])[C:4](=[O:27])[C:5]2[NH:6][C:7]([C:11]3[CH:12]=[N:13][N:14]([CH2:16][C:17]4[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=4)[CH:15]=3)=[N:8][C:9]=2[N:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 222AmmoniaHCID 668032942-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one

생성물 1

HCID 469132692-Amino-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one수율 41%

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온도
127.5 °C

실험 절차

A mixture of 2-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (0.2 g, 0.45 mmol) (prepared as given in Example 1), ammonia solution (20 ml) was heated at 125-130° C. in a sealed tube for 5 days. Reaction mixture was cooled to 0° C. and solid was filtered, washed with methanol, dried and purified by column chromatography using silica gel (100-200 mesh) and 6 to 8% methanol in DCM as an eluent to obtain 2-Amino-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (0.079 g, 41%) as a white solid.

후처리

  1. customReaction mixture
  2. temperaturewas cooled to 0° C.
  3. filtrationsolid was filtered
  4. washwashed with methanol
  5. customdried
  6. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-966f7e3a05d54a1eb51ca12b3b08b1d6
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09284316B2

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