Dimethylformamide → HCID 11702516, 화합물

HRID 2222078노트

반응식

HRID 2222078 반응식
[F:1][C:2]([F:22])([F:21])[C:3]1[N:11]=[C:10]([NH:12][CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:9]=[C:8]2[C:4]=1[NH:5][CH:6]=[N:7]2.[CH3:23]N(C=O)C>>[F:22][C:2]([F:1])([F:21])[C:3]1[N:11]=[C:10]([NH:12][CH2:13][CH2:14][C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:9]=[C:8]2[C:4]=1[N:5]=[CH:6][N:7]2[CH3:23]

참가 물질

3

반응물 2

HCID 6228DimethylformamideHCID 115223956-Trifluoromethyl-2-phenethylaminopurine2회

생성물 1

HCID 11702516HCID 11702516, 화합물수율 80.3%

실험 절차

To a solution of 6-Trifluoromethyl-2-phenethylaminopurine (compound 9, 0.600 g, 1.95 mmol) in DMF (14 ml) K2CO3 (0.351 g, 2.54 mmol) and Mel (0.158 ml, 2.54 mmol) were added. The mixture was stirred at room temperature and after 0.5 h the reaction was complete (HPLC: Rt,product=4.1). Crystallization occurred after the slow addition of water (17 ml). After stirring for 0.5 h the mixture was filtrated and the residue was washed with four 10-ml portions of water. The filtrate was again filtrated after 1 h and the residue was washed with three 5-ml portions of water. The residue was dried in vacuo at 60° C. obtaining the product as a white solid (503 mg, 80%).

후처리

  1. customCrystallization
  2. additionafter the slow addition of water (17 ml)
  3. stirringAfter stirring for 0.5 h the mixture
  4. filtrationwas filtrated
  5. washthe residue was washed with four 10-ml portions of water
  6. filtrationThe filtrate was again filtrated after 1 h
  7. washthe residue was washed with three 5-ml portions of water
  8. customThe residue was dried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-bd86f82e47ab4d5c915f7e3242fc0683
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07371737B2

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