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

HRID 2413515노트

반응식

HRID 2413515 반응식
[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

참가 물질

6

반응물 4

HCID 62649Sodium sulfate decahydrateHCID 166653HydrideHCID 13536441HCID 13536441, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-cf70309ff09a49eabf2c52b75795e070
출처 데이터셋
uspto-grants-1988_01
특허 번호
US04718936

반응 노트

불러오는 중…