Ammonia → HCID 178509056, 화합물

HRID 2269063노트

반응식

HRID 2269063 반응식
[NH2:1][C:2]1[N:10]=[C:9]([SH:11])[N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([OH:19])[N:6]2[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:27][CH2:28][S:29][CH2:30][CH2:31][OH:32].Cl.N>CN(C)C=O>[NH2:1][C:2]1[N:10]=[C:9]([S:11][CH2:27][CH2:28][S:29][CH2:30][CH2:31][OH:32])[N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([OH:19])[N:6]2[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

7

반응물 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 127372-((2-Chloroethyl)thio)ethanolHCID 1785090596-Amino-9-benzyl-8-hydroxy-2-mercaptopurine

생성물 1

HCID 178509056HCID 178509056, 화합물수율 9.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Crude 6-amino-9-benzyl-8-hydroxy-2-mercaptopurine (134 mg, 0.49 mmol) was suspended in dimethylformamide (50 ml). To the suspension were added potassium carbonate (100 mg, 0.73 mmol) and 2-(2-chloroethyl)thioethanol (170 mg, 1.2 mmol) in order. The mixture was stirred at room temperature for 24 hours. To the reaction mixture were added 2N hydrochloric acid and then 28% aqueous ammonia. The mixture was extracted with chloroform, the organic layer was dried on magnesium sulfate and then the solvent was removed in vacuo. The residue was purified by silica gel chromatography (5% methanol/chloroform) to give the subject compound (17 mg, yield 6%).

후처리

  1. extractionThe mixture was extracted with chloroform
  2. customthe organic layer was dried on magnesium sulfate
  3. customthe solvent was removed in vacuo
  4. customThe residue was purified by silica gel chromatography (5% methanol/chloroform)

출처 및 근거

ORD 기록
ord-5425577b15ef41598535a337e6072e6f
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329381B1

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