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N-[2-[(2-chloro-9-cyclopentyl-9H-purin-6-yl)-amino]ethyl]-4-fluoro-benzamide → HCID 178478738, 화합물

HRID 1272678
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HRID 1272678 반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:11]2[CH2:15][CH2:14][CH2:13][CH2:12]2)=[C:4]([NH:16][CH2:17][CH2:18][NH:19][C:20](=[O:28])[C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[N:3]=1.[NH2:29][C@H:30]1[CH2:35][CH2:34][C@H:33]([NH2:36])[CH2:32][CH2:31]1>>[ClH:1].[ClH:1].[NH2:29][C@H:30]1[CH2:35][CH2:34][C@H:33]([NH:36][C:2]2[N:10]=[C:9]3[C:5]([N:6]=[CH:7][N:8]3[CH:11]3[CH2:15][CH2:14][CH2:13][CH2:12]3)=[C:4]([NH:16][CH2:17][CH2:18][NH:19][C:20](=[O:28])[C:21]3[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=3)[N:3]=2)[CH2:32][CH2:31]1
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참가 물질

3

반응물 2

HCID 21922952N-[2-[(2-chloro-9-cyclopentyl-9H-purin-6-yl)-amino]ethyl]-4-fluoro-benzamideHCID 178511674HCID 178511674, 화합물

생성물 1

HCID 178478738HCID 178478738, 화합물

반응 조건

온도
140 °C

실험 절차

247 mg of the product obtained in Stage 1 above and 350 mg of trans-1,4-diaminocyclohexane are mixed together and the reaction medium is heated to 140° C. for 6 hours. After evaporating the solvent, chromatography on silica is carried out (eluent methylene chloride/methanol/ammonium hydroxide 85/15/1.5) followed by taking up in an ethanolic solution of hydrochloric acid, leaving to crystallize, separating, drying under reduced pressure and 130 mg of expected product is recovered.

후처리

  1. customAfter evaporating the solvent, chromatography on silica
  2. customleaving
  3. customto crystallize
  4. customseparating
  5. dry with materialdrying under reduced pressure and 130 mg of expected product
  6. customis recovered

출처 및 근거

ORD 기록
ord-7caaa6f46b634da6ba14736cf5ac838e
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07208598B2

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