Sodium sulfate decahydrate → N-(3-Thienylmethyl)-9H-purin-6-amine

HRID 2413515ノート

反応式

HRID 2413515 の反応式
[CH:1]1[S:5][CH:4]=[CH:3][C:2]=1[C:6]([NH:8][C:9]1[N:17]=[CH:16][N:15]=[C:14]2[C:10]=1[NH:11][CH:12]=[N:13]2)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[S:5]1[CH:4]=[CH:3][C:2]([CH2:6][NH:8][C:9]2[N:17]=[CH:16][N:15]=[C:14]3[C:10]=2[NH:11][CH:12]=[N:13]3)=[CH:1]1

参加物

6

反応物 4

HCID 62649Sodium sulfate decahydrateHCID 166653HydrideHCID 13536441HCID 13536441、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 13536440N-(3-Thienylmethyl)-9H-purin-6-amine収率 25%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A suspension of 20 g (0.082 mole) of 6-(3-thenoylamino)-purine in 1 l of absolute tetrahydrofuran is added dropwise to a stirred suspension of 6.5 g (0.17 mole) of lithium aluminum hydride in 350 ml of absolute tetrahydrofuran at 80° C. After 3 hours, the excess hydride is decomposed with sodium sulfate decahydrate, the residue is filtered off, the filtrate is brought to dryness and the resulting oily crystal slurry is crystallized several times from tetrahydrofuran. 6-(3-Thienylmethylamino)-purine is obtained in a yield of 25%.

後処理

  1. filtrationthe residue is filtered off
  2. customthe resulting oily crystal slurry is crystallized several times from tetrahydrofuran

出典と根拠

ORDレコード
ord-cf70309ff09a49eabf2c52b75795e070
出典データセット
uspto-grants-1988_01
特許番号
US04718936

反応ノート

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