Potassium Carbonate → Ethyl (3-amino-6,8-dioxo-7-propyl-4H,6H-pyrimido[6,1-b][1,3]thiazine-2-yl)carboxylate

HRID 1090652노트

반응식

HRID 1090652 반응식
Cl[C:2]1[N:7]([CH2:8][C:9]#[N:10])[C:6](=[O:11])[N:5]([CH2:12][CH2:13][CH3:14])[C:4](=[O:15])[CH:3]=1.[C:16]([O:20][CH2:21][CH3:22])(=[O:19])[CH2:17][SH:18].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:10][C:9]1[CH2:8][N:7]2[C:6](=[O:11])[N:5]([CH2:12][CH2:13][CH3:14])[C:4](=[O:15])[CH:3]=[C:2]2[S:18][C:17]=1[C:16]([O:20][CH2:21][CH3:22])=[O:19]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12185Ethyl ThioglycolateHCID 150275436-Chloro-1-cyanomethyl-3-propylpyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 15027666Ethyl (3-amino-6,8-dioxo-7-propyl-4H,6H-pyrimido[6,1-b][1,3]thiazine-2-yl)carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 6-chloro-1-cyanomethyl-3-propylpyrimidine-2,4(1H,3H)-dione (1.5 g), ethyl thioglycolate (0.88 g) and potassium carbonate (1 g) in ethanol (30 ml) was refluxed for 15 hours. The reaction solution was concentrated to dryness, and the resulting residue was purified by column chlomatography on silica gel. The resulting crude crystals were recrystalized from ethyl acetate-hexane to give colorless plates (0.23 g, 11%).

후처리

  1. concentrationThe reaction solution was concentrated to dryness
  2. customthe resulting residue was purified by column chlomatography on silica gel
  3. customThe resulting crude crystals were recrystalized from ethyl acetate-hexane
  4. customto give colorless plates (0.23 g, 11%)

출처 및 근거

ORD 기록
ord-c0539ff182a64942881b864be5abe4e6
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05082838

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