3-Chloro-2-trifluoromethylbenzoic acid → HCID 118162167, 화합물

HRID 1749488노트

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HRID 1749488 반응식
[Cl:1][C:2]1[C:3]([C:11]([F:14])([F:13])[F:12])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5](O)=[O:6]>C1COCC1>[Cl:1][C:2]1[C:3]([C:11]([F:12])([F:13])[F:14])=[C:4]([CH2:5][OH:6])[CH:8]=[CH:9][CH:10]=1

참가 물질

3

반응물 1

HCID 116586373-Chloro-2-trifluoromethylbenzoic acid

생성물 1

HCID 118162167HCID 118162167, 화합물수율 85.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
75 °C

실험 절차

To a solution of 3-chloro-2-(trifluoromethyl)benzoic acid (0.15 g, 0.668 mmol) in THF (5 mL) was added dropwise a solution of borane dimethyl sulfide complex in THF (2 M, 0.70 mL, 1.40 mmol) at 0° C. to 5° C. The resulting solution was heated at 75° C. for 2 h under nitrogen atmosphere. The reaction was quenched with MeOH (1 mL) at 0° C. and concentrated under vacuum to give the crude title product (0.12 g). 1H NMR (400 MHz, CDCl3) δ (ppm) 7.66-7.64 (m, 1H), 7.48-7.44 (m, 2H), 4.90 (d, J=2.0 Hz, 2H), 3.70 (t, J=2.0 Hz, 1H).

후처리

  1. customThe reaction was quenched with MeOH (1 mL) at 0° C.
  2. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-afad6e60ea7640f6b33cbf75e9fe556e
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156798B2

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