Difluoromethane → 2-Amino-4-chloro-6-difluoromethoxy-pyrimidine

HRID 1719599

反応式

HRID 1719599 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4](Cl)[N:3]=1.[O:10]1CCOCC1.[F:16][CH2:17][F:18]>[OH-].[Na+]>[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([O:10][CH:17]([F:18])[F:16])[N:3]=1

参加物

5

反応物 3

HCID 6345DifluoromethaneHCID 312751,4-DioxaneHCID 655222-Amino-4,6-dichloropyrimidine

生成物 1

HCID 201856892-Amino-4-chloro-6-difluoromethoxy-pyrimidine

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A suspension of 16.4 g of 2-amino-4,6-dichloro-pyrimidine in 100 ml of 40% sodium hydroxide solution is stirred for 1 hour at a temperature of 95° to 100° C. After the addition of 200 ml of dioxane, there are added at a temperature of 70° to 75° C., within 1 hour, 20 g of gaseous difluoromethane. The organic phase is separated, and concentrated to about 1/5 of its volume; it is then poured into water and the solid precipitate is removed. The yield is 6 g of 2-amino-4-chloro-6-difluoromethoxy-pyrimidine, m.p. 118° to 119° C. (compound No. 1.7).

後処理

  1. additionare added at a temperature of 70° to 75° C., within 1 hour
  2. customThe organic phase is separated
  3. concentrationconcentrated to about 1/5 of its volume
  4. additionit is then poured into water
  5. customthe solid precipitate is removed

出典と根拠

ORDレコード
ord-eadd1abc33df4da4934e63856510af96
出典データセット
uspto-grants-1985_09
特許番号
US04540782

関連ノート

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