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Allylamine → HCID 15908139, 화합물

HRID 1250679
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HRID 1250679 반응식
[C:1]([NH:5][C:6]1[C:7]2[S:15][CH:14]=[C:13]([CH2:16][CH2:17][CH3:18])[C:8]=2[N:9]=[C:10](Cl)[N:11]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:19]([NH2:22])[CH:20]=[CH2:21].C(=O)([O-])O.[Na+]>>[CH2:19]([NH:22][C:10]1[N:11]=[C:6]([NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])[C:7]2[S:15][CH:14]=[C:13]([CH2:16][CH2:17][CH3:18])[C:8]=2[N:9]=1)[CH:20]=[CH2:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7853AllylamineHCID 516892Sodium BicarbonateHCID 15908138HCID 15908138, 화합물

생성물 1

HCID 15908139HCID 15908139, 화합물수율 76.5%

실험 절차

173 mg (0.61 mmol) of 4-t-butylamino-2-chloro-7-propylthieno[3,2-d]pyrimidine and 557 mg (9.8 mmol) of allylamine were heated in a sealed tube at 140° C. for 16 hours. After completion of the reaction, the reaction mixture was allowed to resume room temperature, followed by adding a saturated aqueous sodium hydrogen carbonate solution thereto and extraction with ethyl acetate (50 ml×2). After the organic layer was washed with brine and dried over anhydrous sodium sulfate, the solvent was distilled off. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/4) to give 142 mg (yield: 76.3%) of the title compound.

후처리

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

출처 및 근거

ORD 기록
ord-ed51f85f858e448fb8b6a8332d5d65e4
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06339089B2

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