Sodium Hydroxide → HCID 66801910、化合物

HRID 2366306ノート

反応式

HRID 2366306 の反応式
[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]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 66801766HCID 66801766、化合物

生成物 1

HCID 66801910HCID 66801910、化合物収率 95%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-9d3f6550362d4bc788169047922c66e8
出典データセット
uspto-grants-2014_04
特許番号
US08697708B2

反応ノート

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