Sodium Hydroxide → HCID 66801910, 화합물

HRID 2366306노트

반응식

HRID 2366306 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 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of dimethyl 2-chloro-6-fluoroterephthalate (6.19 g, 25.1 mmol) in tetrahydrofuran (75 mL) was added a solution of 1 N NaOH (27.6 mmol, 27.6 mL). The reaction mixture was stirred at room temperature for 30 min. After the volatiles were removed under reduced pressure, water (30 mL) was added. The aqueous solution was acidified with 1 N HCl to pH 3.0. A white solid precipitated and was collected by filtration, washed with water and diethyl ether, dried in high vacuum to afford the title compound as a white solid (5.54 g, 95% yield). 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+) 233.0 [M+H]+.

후처리

  1. customAfter the volatiles were removed under reduced pressure, water (30 mL)
  2. additionwas added
  3. customA white solid precipitated
  4. filtrationwas collected by filtration
  5. washwashed with water and diethyl ether
  6. customdried in high vacuum

출처 및 근거

ORD 기록
ord-9d3f6550362d4bc788169047922c66e8
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697708B2

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