Hydrochloric Acid → 4-Chloro-3',5'-difluoro-6-(1-hydroxyethyl)-3-methylbiphenyl-2-carboxylic acid

HRID 1499724노트

반응식

HRID 1499724 반응식
[Cl:1][C:2]1[C:3]([CH3:21])=[C:4]([CH:19]=[O:20])[C:5]([C:11]2[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[CH:12]=2)=[C:6]([CH:8]([OH:10])[CH3:9])[CH:7]=1.[OH-:22].[Na+].Cl>CO.O>[Cl:1][C:2]1[C:3]([CH3:21])=[C:4]([C:19]([OH:22])=[O:20])[C:5]([C:11]2[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[CH:12]=2)=[C:6]([CH:8]([OH:10])[CH3:9])[CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 866776594-Chloro-3',5'-difluoro-6-(1-hydroxyethyl)-3-methylbiphenyl-2-carbaldehyde

생성물 1

HCID 866776604-Chloro-3',5'-difluoro-6-(1-hydroxyethyl)-3-methylbiphenyl-2-carboxylic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

To a solution of 4-chloro-3′,5′-difluoro-6-(1-hydroxyethyl)-3-methylbiphenyl-2-carbaldehyde (1.00 g, 3.22 mmol) in methanol (40 mL) was added 1.0 M sodium hydroxide in water (16 mL, 16 mmol), followed by 1.0 M sodium hydroxide in water. After stirred at rt overnight, the mixture was slowly acidified to pH 5 with 1 N HCl, then extracted with EtOAc. The combined organic layers were washed with brine, dried over magnesium sulfate, and concentrated to dry under reduced pressure. The crude residue was used directly in next step (1.05 g, 100%).

후처리

  1. extractionextracted with EtOAc
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customto dry under reduced pressure

출처 및 근거

ORD 기록
ord-fd81364390794106aa383305c1a2cae7
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09199982B2

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