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Sodium Hydroxide → HCID 58083439, 화합물

HRID 2404336
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HRID 2404336 반응식
[OH-].[Na+].[Cl:3][C:4]1[CH:9]=[C:8]([C:10]([O:12]C)=[O:11])[CH:7]=[CH:6][C:5]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[C:20]([F:23])([F:22])[F:21]>CO>[Cl:3][C:4]1[CH:9]=[C:8]([C:10]([OH:12])=[O:11])[CH:7]=[CH:6][C:5]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[C:20]([F:21])([F:22])[F:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 66718347Methyl 2-chloro-2'-(trifluoromethyl)biphenyl-4-carboxylate

생성물 1

HCID 58083439HCID 58083439, 화합물수율 93%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 5N aqueous solution of NaOH (4 mL, 20 mmol) was added into a solution of methyl 2-chloro-2′-(trifluoromethyl)biphenyl-4-carboxylate (1.07 g, 3.40 mmol) in MeOH (16 mL) and stirred at RT for 30 minutes. The reaction mixture was concentrated under vacuum. The residue was taken up with EtOAc and washed with a 1N aqueous solution of HCl (3×) and brine, and then dried (MgSO4) and concentrated under vacuum to give the title compound as a white powder (950 mg, 93%). HPLC (Method A) Rt 4.9 min (Purity: 99.4%). LC/MS (Method B): 299.1 (M−H)−. 1H NMR (DMSO-d6, 300 MHz) δ 13.48 (s, 1H), 8.03 (d, J=1.6 Hz, 1H), 7.94 (dd, J=7.9, 1.6 Hz, 1H), 7.89 (d, J=7.8 Hz, 1H), 7.78 (m, 1H), 7.69 (m, 1H), 7.49 (d, J=7.9 Hz, 1H), 7.41 (d, J=7.4 Hz, 1H).

후처리

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. washwashed with a 1N aqueous solution of HCl (3×) and brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-673507b35e6b4c57abb9b3aa47c9258e
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08802704B2

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