Allylamine → HCID 18326381, 화합물

HRID 1250626

반응식

HRID 1250626 반응식
[CH2:1]([N:4]([CH2:16][CH:17]=[CH2:18])[C:5]1[C:6]2[S:14][CH:13]=[C:12]([CH3:15])[C:7]=2[N:8]=[C:9]([Cl:11])[N:10]=1)[CH:2]=[CH2:3].[CH2:19]([NH2:22])[CH:20]=[CH2:21].C(=O)([O-])O.[Na+]>>[ClH:11].[CH2:19]([NH:22][C:9]1[N:10]=[C:5]([N:4]([CH2:16][CH:17]=[CH2:18])[CH2:1][CH:2]=[CH2:3])[C:6]2[S:14][CH:13]=[C:12]([CH3:15])[C:7]=2[N:8]=1)[CH:20]=[CH2:21]

참가 물질

4

반응물 3

HCID 7853AllylamineHCID 516892Sodium BicarbonateHCID 183265134-Diallylamino-2-chloro-7-methylthieno[3,2-d]pyrimidine

생성물 1

HCID 18326381HCID 18326381, 화합물

실험 절차

In a sealed tube were heated 335 mg (1.2 mmol) of 4-diallylamino-2-chloro-7-methylthieno[3,2-d]pyrimidine and 1.10 g (19.2 mmol) of allylamine at 140° C. for 16 hours. After completion of the reaction, the reaction mixture was allowed to resume room temperature, and a saturated aqueous sodium hydrogen carbonate solution was added thereto, followed by extraction with ethyl acetate (50 ml×2). The organic layer was washed with brine and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4) to give 277 mg (yield: 77.0%) of a free base compound of the title compound.

후처리

  1. customAfter completion of the reaction
  2. customto resume room temperature
  3. extractionfollowed by extraction with ethyl acetate (50 ml×2)
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4)

출처 및 근거

ORD 기록
ord-d2f5b77e193f40aa827759bc873706ba
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06339089B2

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