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Acrylamide → HCID 86684910, 화합물

HRID 2402903
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HRID 2402903 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1.[C:13]([NH2:17])(=[O:16])[CH:14]=[CH2:15].B([O-])([O-])[O-].B([O-])([O-])[O-].B([O-])([O-])[O-].B([O-])([O-])[O-].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+]>CO.O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:15][CH2:14][C:13]([NH2:17])=[O:16])=[C:4]([C:9]([F:12])([F:10])[F:11])[CH:3]=1
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참가 물질

6

반응물 3

HCID 6579AcrylamideHCID 21225931Dodecasodium;tetraborateHCID 509979974-Bromo-2-(trifluoromethyl)benzenethiol

생성물 1

HCID 86684910HCID 86684910, 화합물수율 98.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water
용매

실험 절차

4-Bromo-2-trifluoromethyl-benzenethiol (259.2 g, 1.01 mol) was dissolved in methanol (1.3 L) and water (2.6 L), then acrylamide (130 g, 1.82 mol), followed by sodium tetraborate (25.9 g, 129 mmol) were added at room temperature. The suspension was stirred for 40 h. After filtration, the solid was washed with water (2.6 L) and n-heptane (2.6 L) and dried in vacuo to yield the title compound as a white powder (325.6 g, 98%). MS (EI): m/z=330.0, 328.0 [M+H]+. 1H NMR (d6-DMSO, 400 MHz): δ 2.40 (t, J=7.2 Hz, 2H), 3.24 (t, J=7.2 Hz, 2H), 6.92 (bs, 1H), 7.37 (bs, 1H), 7.60 (d, J=8.3 Hz, 1H), 7.82-7.88 (m, 2H).

후처리

  1. additionwere added at room temperature
  2. filtrationAfter filtration
  3. washthe solid was washed with water (2.6 L) and n-heptane (2.6 L)
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-1290d83fcca34f5992c7fb9ea4052f27
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796471B2

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