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Ethylene Glycol → HCID 69070807, 화합물

HRID 388399
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인쇄 미리보기

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HRID 388399 반응식
Cl[CH2:2][C:3]1[NH:4][C:5](=[O:18])[C:6]2[C:11]([CH3:12])=[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[S:9][C:7]=2[N:8]=1.[C:19]([O:23][C:24]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)=[O:25])([CH3:22])([CH3:21])[CH3:20].C(O)CO.C(N(CC)CC)C>O>[C:19]([O:23][C:24]([N:26]1[CH2:31][CH2:30][N:29]([CH2:2][C:3]2[NH:4][C:5](=[O:18])[C:6]3[C:11]([CH3:12])=[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[S:9][C:7]=3[N:8]=2)[CH2:28][CH2:27]1)=[O:25])([CH3:22])([CH3:20])[CH3:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 2339310ethyl 2-(chloromethyl)-5-methyl-4-oxo-3H,4H-thieno[2,3-d]pyrimidine-6-carboxylate

생성물 1

HCID 69070807HCID 69070807, 화합물수율 78%

시약·촉매·용매 1

HCID 962
Water
용매

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온도
80 °C

실험 절차

A mixture of 1.15 g of ethyl 2-chloromethyl-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate, 745 mg of tert-butoxycarbonylpiperazine, 20 mL of ethylene glycol and 400 mg of triethylamine was stirred at 80° C. for 3 hours. Thereafter water was added to the reaction mixture, followed by extraction with chloroform, drying over anhydrous magnesium sulfate, and removal of the solvent by distillation under reduced pressure. The residue was purified on silica gel column chromatography (ethyl acetate:chloroform:hexane=2:1:1) to provide 1.36 g (78%) of the title compound.

후처리

  1. extractionfollowed by extraction with chloroform
  2. dry with materialdrying over anhydrous magnesium sulfate, and removal of the solvent by distillation under reduced pressure
  3. customThe residue was purified on silica gel column chromatography (ethyl acetate:chloroform:hexane=2:1:1)

출처 및 근거

ORD 기록
ord-b7eac9cb316b47908e74de8e780c5b58
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08377944B2

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