Ethanol → (3-(((2-Amino-6-chloro-4-pyrimidinyl)amino)methyl)-3-oxetanyl)methanol

HRID 1421872노트

반응식

HRID 1421872 반응식
[NH2:1][CH2:2][C:3]1([CH2:7][OH:8])[CH2:6][O:5][CH2:4]1.[NH2:9][C:10]1[N:15]=[C:14](Cl)[CH:13]=[C:12]([Cl:17])[N:11]=1.C(O)C>C(N(CC)CC)C>[NH2:9][C:10]1[N:15]=[C:14]([NH:1][CH2:2][C:3]2([CH2:7][OH:8])[CH2:6][O:5][CH2:4]2)[CH:13]=[C:12]([Cl:17])[N:11]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 655222-Amino-4,6-dichloropyrimidineHCID 18706850[3-(Aminomethyl)oxetan-3-yl]methanol

생성물 1

HCID 385214(3-(((2-Amino-6-chloro-4-pyrimidinyl)amino)methyl)-3-oxetanyl)methanol수율 32.8%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A mixture of 3-aminomethyl-3-hydroxymethyloxetane (1.17 g, 0.01 mol), 2-amino-4,6-dichloropyrimidine (1.64 g, 0.01 mol), ethanol (40 ml) and triethylamine (4 ml) was refluxed for one day. The solvent was distilled away under reduced pressure and ethyl acetate was added to the residue. The mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=20:1, later 10:1) to give colorless prism crystals (0.8 g, 32.8%), m.p. 185-186° C. (acetone).

후처리

  1. temperaturewas refluxed for one day
  2. distillationThe solvent was distilled away under reduced pressure and ethyl acetate
  3. additionwas added to the residue
  4. washThe mixture was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled away under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (chloroform

출처 및 근거

ORD 기록
ord-efe1ab6d86274af3afad69431d791d0c
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080750

반응 노트

불러오는 중…