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

HRID 1633343

반응식

HRID 1633343 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

A suspension of 16.4 g of 2-amino-4,6-dichloropyrimidine 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).

후처리

  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

출처 및 근거

ORD 기록
ord-f9b034d86e7a4f48988df82a1abb1b11
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04480101

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