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Allylamine → HCID 15908144, 화합물

HRID 1250683
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HRID 1250683 반응식
[CH2:1]([NH:4][C:5]1[C:6]2[S:14][CH:13]=[C:12]([CH:15]([CH3:17])[CH3:16])[C:7]=2[N:8]=[C:9](Cl)[N:10]=1)[CH:2]=[CH2:3].[CH2:18]([NH2:21])[CH:19]=[CH2:20].C(=O)([O-])O.[Na+]>>[CH2:18]([NH:21][C:9]1[N:10]=[C:5]([NH:4][CH2:1][CH:2]=[CH2:3])[C:6]2[S:14][CH:13]=[C:12]([CH:15]([CH3:17])[CH3:16])[C:7]=2[N:8]=1)[CH:19]=[CH2:20]
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참가 물질

4

반응물 3

HCID 7853AllylamineHCID 516892Sodium BicarbonateHCID 15908143HCID 15908143, 화합물

생성물 1

HCID 15908144HCID 15908144, 화합물수율 89.3%

실험 절차

70 mg (0.26 mmol) of 4-allylamino-2-chloro-7-isopropylthieno[3,2-d]pyrimidine and 239 mg (4.2 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 (30 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 67 mg (yield: 89.3%) of the title compound.

후처리

  1. customAfter completion of the reaction
  2. customto resume room temperature
  3. extractionextraction with ethyl acetate (30 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-c4d69a6e42fb450080a060727a3f50ff
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06339089B2

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