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Carbon tetrabromide → HCID 67358461, 화합물

HRID 1667200
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HRID 1667200 반응식
[CH3:1][C:2]1[N:3]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)[S:5][C:6]=1[CH2:7]O.C(Br)(Br)(Br)[Br:20].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[Br:20][CH2:7][C:6]1[S:5][C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)=[N:3][C:2]=1[CH3:1]
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참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 22647518{4-Methyl-2-[3-(trifluoromethyl)phenyl]-1,3-thiazol-5-yl}methanol

생성물 1

HCID 67358461HCID 67358461, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of {4-methyl-2-[3-(trifluoromethyl)phenyl]-1,3-thiazol-5-yl}methanol (90.2 g, 0.732 mmol) in dichloromethane (10 mL) was added carbon tetrabromide (0.485 g, 1.464 mmol) and triphenylphosphine (0.384 g, 1.464 mmol). The reaction mixture was then stirred at room temperature for 16 hours. The reaction mixture was concentrated, and the residue was chromatographed on silica gel eluting with 10-20% ethyl acetate/hexane to yield the title compound. 1H NMR (300 MHz, CDCl3) δ ppm 8.18 (s, 1H), 8.06 (d, J=7.54 Hz, 1H), 7.67 (d, 1H), 7.56 (t, J=7.73 Hz, 1H), 4.72 (m, 2H), 2.48 (m, 3H).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue was chromatographed on silica gel eluting with 10-20% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-734979f180c04c2cad7aff557bb15bbe
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044069B2

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