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2-chloro-N-phenyl-9-(tetrahydro-3-thienyl)-9H-purin-6-amine → N2-(4-aminocyclo-hexyl)-N6-phenyl-9-(tetrahydro-3-thienyl)-9H-purin-2,6-diamine Dihydrochloride

HRID 1244913
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HRID 1244913 반응식
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH2:8])[CH2:4][CH2:3]1.[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([N:14]=[CH:15][N:16]2[CH:19]2[CH2:23][CH2:22][S:21][CH2:20]2)=[C:12]([NH:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[N:11]=1>>[ClH:9].[ClH:9].[NH2:1][CH:2]1[CH2:7][CH2:6][CH:5]([NH:8][C:10]2[N:18]=[C:17]3[C:13]([N:14]=[CH:15][N:16]3[CH:19]3[CH2:23][CH2:22][S:21][CH2:20]3)=[C:12]([NH:24][C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[N:11]=2)[CH2:4][CH2:3]1
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참가 물질

3

반응물 2

HCID 219229282-chloro-N-phenyl-9-(tetrahydro-3-thienyl)-9H-purin-6-amineHCID 178511674HCID 178511674, 화합물

생성물 1

HCID 18457589N2-(4-aminocyclo-hexyl)-N6-phenyl-9-(tetrahydro-3-thienyl)-9H-purin-2,6-diamine Dihydrochloride수율 127.9%

실험 절차

The operation is carried out as in Stage 3 of Example 5 starting from 536 mg of trans-1,4-diaminocyclohexane and 156 mg of the product obtained in Stage 1 above, the reaction medium is taken to a temperature of approximately 140 to 145° C. for approximately 4 hours 30 minutes then left to return to ambient temperature. After purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2 salification is carried out with 1.4 N hydrochloric acid in ethanol, followed by separating, washing and drying at a temperature of approximately 50° C. In this way 145 mg of expected product is obtained in the form of pink beige crystals.

후처리

  1. waitthen left
  2. customto return to ambient temperature
  3. customAfter purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2 salification
  4. customby separating
  5. washwashing
  6. customdrying at a temperature of approximately 50° C

출처 및 근거

ORD 기록
ord-2ed82099136b4f288565db76e544fda5
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122669B1

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