Methanol → 3-Hydroxy-5-(trifluoromethyl)thiophene-2-carboxylic acid

HRID 362178노트

반응식

HRID 362178 반응식
[OH:1][C:2]1[CH:6]=[C:5]([C:7]([F:10])([F:9])[F:8])[S:4][C:3]=1[C:11]([O:13]C)=[O:12].CO.[OH-].[Na+]>O>[OH:1][C:2]1[CH:6]=[C:5]([C:7]([F:10])([F:8])[F:9])[S:4][C:3]=1[C:11]([OH:13])=[O:12]

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 2759855Methyl 3-hydroxy-5-(trifluoromethyl)thiophene-2-carboxylate

생성물 1

HCID 27593483-Hydroxy-5-(trifluoromethyl)thiophene-2-carboxylic acid수율 65%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1B (2.38 g) and methanol (20 ml) was added to a stirred solution of sodium hydroxide (1.68 g) in water (20 ml). The reaction mixture was heated at reflux for 3 hours. The reaction mixture was cooled to room temperature and concentrated in vacuo. The concentrate was cooled to 5° C. and acidified with concentrated HCl (3.5 ml). The resulting suspension was stirred at 5° C. for 30 minutes. The solid was collected by filtration, washed with water, then dried in vacuo at 35°-40° C. to give the free acid (1.45 g, 65%).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 3 hours
  3. concentrationconcentrated in vacuo
  4. temperatureThe concentrate was cooled to 5° C.
  5. filtrationThe solid was collected by filtration
  6. washwashed with water
  7. customdried in vacuo at 35°-40° C.

출처 및 근거

ORD 기록
ord-f19a28194f8344e6913d0e72d9d39e84
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05869426

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