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3-Bromo-1,1,1-trifluoro-2-propanone → HCID 67028825, 화합물

HRID 2061869
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HRID 2061869 반응식
[Br:1][C:2]1[C:3]([C:16](=[S:18])[NH2:17])=[CH:4][C:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[N:6][CH:7]=1.C(=O)(O)[O-].[Na+].[F:24][C:25]([F:31])([F:30])[C:26]([CH2:28]Br)=[O:27]>O1CCCC1>[Br:1][C:2]1[C:3]([C:16]2[S:18][CH2:28][C:26]([OH:27])([C:25]([F:31])([F:30])[F:24])[N:17]=2)=[CH:4][C:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:13])([CH3:14])[CH3:12])=[N:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 790083-Bromo-1,1,1-trifluoro-2-propanoneHCID 516892Sodium BicarbonateHCID 86643630HCID 86643630, 화합물2회

생성물 1

HCID 67028825HCID 67028825, 화합물수율 85.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a 2 L round bottom flask was charged tert-butyl 5-bromo-4-carbamothioylpyridin-2-ylcarbamate (Intermediate 85, 50 g, 151 mmol) in tetrahydrofuran (800 mL), then solid sodium bicarbonate (25.4 g, 302 mmol) was added followed by 1,1,1-trifluoro-3-bromoacetone (31 mL, 290 mmol). The resulting mixture (yellow suspension) was allowed to stir at room temperature overnight. The white suspension was filtered and the solid was washed with water (2.2˜2.5 L). The white solid was dried under vacuum to give 56.8g of white powder (85%)

후처리

  1. filtrationThe white suspension was filtered
  2. washthe solid was washed with water (2.2˜2.5 L)
  3. customThe white solid was dried under vacuum

출처 및 근거

ORD 기록
ord-f9f5564c1c2f4f1c8f3a75a0d7e28db4
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283361B2

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