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

HRID 2171479ノート

反応式

HRID 2171479 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59416aa5f5b547bab0f7a134fa85eb0e
出典データセット
uspto-grants-2015_06
特許番号
US09051323B2

反応ノート

読み込み中…