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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 1272634
ノート
印刷プレビュー

反応式

HRID 1272634 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 219229282-chloro-N-phenyl-9-(tetrahydro-3-thienyl)-9H-purin-6-amineHCID 178511674HCID 178511674、化合物

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-faf43d0500834664ad5fac4604d546e1
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07208598B2

反応ノート

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