Sodium Hydroxide → HCID 66801910, 화합물

HRID 449926노트

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HRID 449926 반응식
[Cl:1][C:2]1[CH:11]=[C:10]([C:12]([O:14]C)=[O:13])[CH:9]=[C:8]([F:16])[C:3]=1[C:4]([O:6][CH3:7])=[O:5].[OH-].[Na+]>O1CCCC1>[Cl:1][C:2]1[CH:11]=[C:10]([CH:9]=[C:8]([F:16])[C:3]=1[C:4]([O:6][CH3:7])=[O:5])[C:12]([OH:14])=[O:13]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 66801766HCID 66801766, 화합물

생성물 1

HCID 66801910HCID 66801910, 화합물수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of dimethyl 2-chloro-6-fluoroterephthalate (2.784 g, 11.3 mmoles) in tetrahydrofuran (20 mL) was added a solution of 1 N NaOH (12.4 mmol, 12.4 mL). The reaction mixture was stirred at room temperature for 30 min. The reaction was concentrated under reduced pressure and the residue was suspended in water (10 mL). The aqueous solution was acidified to pH 3 with 1 N HCl. The resulting white precipitate was collected by filtration, washed with water and ether, dried in high vacuum to afford 3-chloro-5-fluoro-4-(methoxycarbonyl)benzoic acid as a white solid (2.52 g, yield: 96%). 1H NMR (400 MHz, CDCl3) δ 7.96 (s, 1H), 7.76 (dd, J=8.8, 1.3 Hz, 1H), 4.01 (s, 3H). LCMS (APCI+) [M+H]+233.0.

후처리

  1. concentrationThe reaction was concentrated under reduced pressure
  2. filtrationThe resulting white precipitate was collected by filtration
  3. washwashed with water and ether
  4. customdried in high vacuum

출처 및 근거

ORD 기록
ord-588e676ff8d74d5e9bae935201a49f17
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486950B2

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