Hydrochloric Acid → 3-Ethyl-5-(3-hydroxy-benzylcarbamoyl)-thiophene-2-carboxylic acid

HRID 1952629노트

반응식

HRID 1952629 반응식
C[O:2][C:3]([C:5]1[S:6][C:7]([C:12](=[O:22])[NH:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([OH:21])[CH:16]=2)=[CH:8][C:9]=1[CH2:10][CH3:11])=[O:4].O.[OH-].[Li+].C1COCC1.Cl>O>[CH2:10]([C:9]1[CH:8]=[C:7]([C:12](=[O:22])[NH:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([OH:21])[CH:16]=2)[S:6][C:5]=1[C:3]([OH:4])=[O:2])[CH3:11]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 682269473-Ethyl-5-(3-hydroxy-benzylcarbamoyl)-thiophene-2-carboxylic acid methyl ester

생성물 1

HCID 682268133-Ethyl-5-(3-hydroxy-benzylcarbamoyl)-thiophene-2-carboxylic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3-Ethyl-5-(3-hydroxy-benzylcarbamoyl)-thiophene-2-carboxylic acid methyl ester (140 mg, 0.44 mmol), lithium hydroxide monohydrate (180 mg, 4.38 mmol), THF (4 mL) and water (5 mL) was stirred 15 h, acidified with 1N HCl and extracted with EtOAc (×3). The organic extracts were combined, washed with brine, dried over sodium sulfate, filtered and evaporated to give the title compound, 145.4 (100%). MS m/e 305.9 (M+H+).

후처리

  1. extractionextracted with EtOAc (×3)
  2. washwashed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-9f4381e654a0412b8d69b81f52fbb6fe
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404859B2

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