Sodium Hydroxide → 6-(N-Allyl-N-cyclohexylamino)-9-(8-carboxyoctyl)-purine

HRID 1721845

反応式

HRID 1721845 の反応式
[CH2:1]([N:4]([C:11]1[N:19]=[CH:18][N:17]=[C:16]2[C:12]=1[N:13]=[CH:14][N:15]2[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]([O:30]C)=[O:29])[CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)[CH:2]=[CH2:3].[OH-].[Na+]>C(O)C>[CH2:1]([N:4]([C:11]1[N:19]=[CH:18][N:17]=[C:16]2[C:12]=1[N:13]=[CH:14][N:15]2[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]([OH:30])=[O:29])[CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)[CH:2]=[CH2:3]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 200299766-(N-Allyl-N-cyclohexylamino)-9-(8-methoxycarbonyloctyl)-purine

生成物 1

HCID 138519416-(N-Allyl-N-cyclohexylamino)-9-(8-carboxyoctyl)-purine収率 71%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3.2 g. (7.5 mmole) of the compound of Example 13 are heated under reflux for 5 hours with 50 ml. 5% aqueous sodium hydroxide solution and 40 ml. ethanol. The reaction mixture is evaporated and the residue is taken up in water, washed with diethyl ether and the aqueous phase is adjusted to pH 6, extracted with dichloromethane, dried and evaporated. After trituration of the residue with diethyl ether, there are obtained 2.2 g. of the title compound (71% of theory); m.p. 100°-102° C.

後処理

  1. temperatureunder reflux for 5 hours with 50 ml
  2. customThe reaction mixture is evaporated
  3. washwashed with diethyl ether
  4. extractionextracted with dichloromethane
  5. customdried
  6. customevaporated
  7. customAfter trituration of the residue with diethyl ether, there are obtained 2.2 g

出典と根拠

ORDレコード
ord-468c9a33d02847a0883d83e37825a367
出典データセット
uspto-grants-1989_08
特許番号
US04853386

関連ノート

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