4-Amino-6-chloro-2-methylthiopyrimidine → 7-Chloro-5-(methylthio)imidazo[1,2-c]pyrimidine

HRID 2171479노트

반응식

HRID 2171479 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.CO[CH:13](OC)[CH2:14]Br>O1CCOCC1.O>[Cl:8][C:6]1[N:5]=[C:4]([S:9][CH3:10])[N:3]2[CH:13]=[CH:14][N:1]=[C:2]2[CH:7]=1

참가 물질

5

반응물 2

HCID 704964-Amino-6-chloro-2-methylthiopyrimidineHCID 816722-Bromo-1,1-dimethoxyethane

생성물 1

HCID 408159747-Chloro-5-(methylthio)imidazo[1,2-c]pyrimidine

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

75 g (427 mmol) of 4-amino-6-chloro-2-(methylthio)pyrimidine are dissolved in 3000 ml of dioxane and 750 ml of water. 101.05 g (597.81 mmol) of bromoacetaldehyde dimethyl acetal are added, and the mixture is heated under reflux for 24 h. After the reaction is complete, the dioxane is removed in vacuo and the aqueous suspension is suspended in THF, filtered with suction and washed with some THF. Drying of the solid at 40° C. under high vacuum results in 56.5 g (66% of theory) of the product.

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 24 h
  3. customthe dioxane is removed in vacuo
  4. filtrationfiltered with suction
  5. washwashed with some THF
  6. customDrying of the solid at 40° C. under high vacuum
  7. customresults in 56.5 g (66% of theory) of the product

출처 및 근거

ORD 기록
ord-59416aa5f5b547bab0f7a134fa85eb0e
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051323B2

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