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

HRID 410000노트

반응식

HRID 410000 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ca2733eec1d54aea9fcfe32777919684
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759542B2

반응 노트

불러오는 중…