Ammonia → 4,5-Pyrimidinediamine, 6-chloro-
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
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- 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
- temperaturethe resulting solution was cooled to rt
- waitto stand for 2 h
- customThe colorless crystalline material that resulted
- filtrationwas collected by filtration
- 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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