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2-chloro-N-[2-[(2-chloro-9-cyclopentyl-9H-purin-6-yl)-amino]-ethyl]-4-nitro-benzamide → HCID 178478741, 화합물

HRID 1244961
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HRID 1244961 반응식
[Cl:1][C:2]1[CH:28]=[C:27]([N+:29]([O-:31])=[O:30])[CH:26]=[CH:25][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][NH:9][C:10]1[N:18]=[C:17](Cl)[N:16]=[C:15]2[C:11]=1[N:12]=[CH:13][N:14]2[CH:20]1[CH2:24][CH2:23][CH2:22][CH2:21]1)=[O:5].[NH2:32][C@H:33]1[CH2:38][CH2:37][C@H:36]([NH2:39])[CH2:35][CH2:34]1>>[ClH:1].[ClH:1].[NH2:32][C@H:33]1[CH2:38][CH2:37][C@H:36]([NH:39][C:17]2[N:16]=[C:15]3[C:11]([N:12]=[CH:13][N:14]3[CH:20]3[CH2:21][CH2:22][CH2:23][CH2:24]3)=[C:10]([NH:9][CH2:8][CH2:7][NH:6][C:4](=[O:5])[C:3]3[CH:25]=[CH:26][C:27]([N+:29]([O-:31])=[O:30])=[CH:28][C:2]=3[Cl:1])[N:18]=2)[CH2:35][CH2:34]1
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참가 물질

3

반응물 2

HCID 219229622-chloro-N-[2-[(2-chloro-9-cyclopentyl-9H-purin-6-yl)-amino]-ethyl]-4-nitro-benzamideHCID 178511674HCID 178511674, 화합물

생성물 1

HCID 178478741HCID 178478741, 화합물

반응 조건

온도
140 °C

실험 절차

295 mg of the product obtained in Stage 1 above and 362 mg of trans-1,4-diaminocyclohexane are mixed together and the reaction medium is heated to approximately 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) then taken up in an ethanolic solution of hydrochloric acid, followed by leaving to crystallize, separating, drying under reduced pressure and 105 mg of expected product is recovered.

후처리

  1. customAfter evaporating the solvent, chromatography on silica
  2. customby leaving
  3. customto crystallize
  4. customseparating
  5. dry with materialdrying under reduced pressure and 105 mg of expected product
  6. customis recovered

출처 및 근거

ORD 기록
ord-fbc7bad90db947b1b69943a18c3451ed
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122669B1

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