Water → 3-amino-5-(4-fluorophenyl)thiophene-2-carboxylic Acid

HRID 460318

반응식

HRID 460318 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)[S:4][C:3]=1[C:14]([O:16]C)=[O:15].[OH-].[Li+].O.C1COCC1>CO>[NH2:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([F:13])=[CH:11][CH:12]=2)[S:4][C:3]=1[C:14]([OH:16])=[O:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 619692Methyl 3-amino-5-(4-fluorophenyl)thiophene-2-carboxylate

생성물 1

HCID 107523413-amino-5-(4-fluorophenyl)thiophene-2-carboxylic Acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The mixture consisting of 500 mg of methyl 3-amino-5-(4-fluorophenyl)thiophene-2-carboxylate, 160 mg of lithium hydroxide, 2 ml of water, 2 ml of THF and 2 ml of methanol is stirred at RT for 3 days. After dilution with 15 ml of water, unhydrolyzed ester is removed by extraction with ethyl acetate. The aqueous phase is adjusted to pH 5 using hydrochloric acid and stirred, and the precipitated solid is filtered off with suction and dried.

후처리

  1. customAfter dilution with 15 ml of water, unhydrolyzed ester is removed by extraction with ethyl acetate
  2. stirringstirred
  3. filtrationthe precipitated solid is filtered off with suction
  4. customdried

출처 및 근거

ORD 기록
ord-2c96ff4f637f4338b0e2cb3a6cd9e194
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196114B2

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