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

HRID 460318

反応式

HRID 460318 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2c96ff4f637f4338b0e2cb3a6cd9e194
出典データセット
uspto-grants-2007_03
特許番号
US07196114B2

関連ノート

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