Ammonia → 4,5-Pyrimidinediamine, 6-chloro-

HRID 60193

반응식

HRID 60193 반응식
[NH3:1].[Cl:2][C:3]1[C:8]([NH2:9])=[C:7](Cl)[N:6]=[CH:5][N:4]=1>CO>[Cl:2][C:3]1[N:4]=[CH:5][N:6]=[C:7]([NH2:1])[C:8]=1[NH2:9]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 794345-Amino-4,6-dichloropyrimidine

생성물 1

HCID 780104,5-Pyrimidinediamine, 6-chloro-수율 71%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
100 °C

실험 절차

To a 7 N solution of ammonia in MeOH (40 mL) was added 4,6-dichloropyrimidin-5-ylamine (8.7 g, 53 mmol) and the solution was heated to 100° C. in a sealed tube. After 12 h, the resulting solution was cooled to rt and allowed to stand for 2 h. The colorless crystalline material that resulted was collected by filtration and washed with ice cold MeOH (10 mL) to give the title compound (5.4 g, 71%). MS (ESI): mass calcd. for C4H5ClN4, 144.0; m/z found, 145.0 [M+H]+. 1H NMR ((CD3)250): 7.64 (s, 1H), 6.70 (s, 2H), 4.93 (s, 2H).

후처리

  1. temperaturethe resulting solution was cooled to rt
  2. waitto stand for 2 h
  3. customThe colorless crystalline material that resulted
  4. filtrationwas collected by filtration
  5. washwashed with ice cold MeOH (10 mL)

출처 및 근거

ORD 기록
ord-6fbcc52a42154b628a7afb18ebbb138a
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440978B2

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