Water → 1-Methyl-3(carboethoxypropyl)-7-(pivaloyloxymethyl)xanthine

HRID 904272

반응식

HRID 904272 반응식
[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[N:9]([CH2:13][O:14][C:15](=[O:20])[C:16]([CH3:19])([CH3:18])[CH3:17])[CH:8]=[N:7][C:6]=2[NH:5][C:3]1=[O:4].C(=O)([O-])[O-].[Na+].[Na+].I[CH2:28][CH2:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32].O>CN(C=O)C.CCO.C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[N:9]([CH2:13][O:14][C:15](=[O:20])[C:16]([CH3:17])([CH3:19])[CH3:18])[CH:8]=[N:7][C:6]=2[N:5]([CH2:28][CH2:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:3]1=[O:4]

참가 물질

7

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 10890062Ethyl 4-iodobutanoateHCID 128798411-Methyl-7-(pivaloyloxymethyl)xanthine

생성물 1

HCID 128798421-Methyl-3(carboethoxypropyl)-7-(pivaloyloxymethyl)xanthine

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 21889567Chloroform ethanol용매

실험 절차

A mixture of 1-methyl-7-(pivaloyloxymethyl)xanthine (350 mg, 1.25 mmes ) sodium carbonate (265 mg, 2.50 mmoles) and ethyl 4-iodobutyrate(384 μl, 2.50 mmole) in 5.8 ml dry DMF was stirred under nitrogen at room temperature for 18 hours. Water was added and the reaction mixture extracted with chloroform. After drying, the extracts were stripped to leave a yellow oil which goes to chromotographed on four thick silica gel plates with 10% EtOH/CHCl3. The band was scraped off and eluted with 100 ml of 25% EtOH/CHCl3 to yield 609 ml of the desired product as an oil.

후처리

  1. extractionthe reaction mixture extracted with chloroform
  2. customAfter drying
  3. customto leave a yellow oil which
  4. washeluted with 100 ml of 25% EtOH/CHCl3

출처 및 근거

ORD 기록
ord-48aa61996d4241aeaec20ac03e45d158
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04230805

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