Hydrochloric Acid → 4-[(2-Fluorobenzyl)oxy]benzoic acid

HRID 410000ノート

反応式

HRID 410000 の反応式
[F:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([O:12]C)=[O:11])=[CH:8][CH:7]=1.[OH-].[K+].Cl>CO.C1COCC1>[F:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([OH:12])=[O:11])=[CH:8][CH:7]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19861855Methyl 4-[(2-fluorophenyl)methoxy]benzoate

生成物 1

HCID 64628464-[(2-Fluorobenzyl)oxy]benzoic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 4-(2-fluorobenzyloxy)benzoate (P1, 10.0 g, 26.9 mmol) was dissolved in methanol (60 mL) and THF (90 mL). A 45 wt % potassium hydroxide solution (20 mL) was then added and the resulting exotherm was controlled by a water bath. After 1.5 days at 20-25° C. the solution became a thick suspension. Using a water bath to control the exotherm, 20 mL of concentrated HCl was added. The mixture was then concentrated to remove the THF and methanol and 150 mL water was added. The solid was isolated by filtration and washed with 50 mL water. After drying under vacuum, the title compound was isolated as a white crystalline solid (9.4 g, 99% yield).

後処理

  1. customthe resulting exotherm was controlled by a water bath
  2. additionwas added
  3. concentrationThe mixture was then concentrated
  4. customto remove the THF and methanol and 150 mL water
  5. additionwas added
  6. customThe solid was isolated by filtration
  7. washwashed with 50 mL water
  8. customAfter drying under vacuum

出典と根拠

ORDレコード
ord-ca2733eec1d54aea9fcfe32777919684
出典データセット
uspto-grants-2014_06
特許番号
US08759542B2

反応ノート

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