Sodium Bicarbonate → HCID 10089559、化合物

HRID 1271846ノート

反応式

HRID 1271846 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([C:17]1[S:21][C:20]2[CH:22]=[CH:23][C:24]([O:26][CH2:27][CH2:28][N:29]([CH3:31])[CH3:30])=[CH:25][C:19]=2[CH:18]=1)=[O:16])(C)(C)C.C(=O)(O)[O-].[Na+]>FC(F)(F)C(O)=O>[NH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([C:17]1[S:21][C:20]2[CH:22]=[CH:23][C:24]([O:26][CH2:27][CH2:28][N:29]([CH3:31])[CH3:30])=[CH:25][C:19]=2[CH:18]=1)=[O:16]

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 69489634HCID 69489634、化合物

生成物 1

HCID 10089559HCID 10089559、化合物収率 63.3%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 72 mg (0.158 mmol) (2-{[5-(2-Dimethylamino-ethoxy)-benzo[b]thiophene-2-carbonyl]-amino}-phenyl)-carbamic acid tert-butyl ester (5) in 1.0 ml trifluoroacetic acid was stirred for 60 min at room temperature and then added to an aqueous solution of sodium bicarbonate. After extraction with ethyl acetate and removal of the solvent the residue was recrystallized from ethyl acetate/diethyl ether to yield 35 mg (0.10 mmol) 5-(2-Dimethylamino-ethoxy)-benzo[b]thiophene-2-carboxylic acid (2-amino-phenyl)-amide (1) as a yellow solid, mp. 191–193° C.

後処理

  1. extractionAfter extraction
  2. customwith ethyl acetate and removal of the solvent the residue
  3. customwas recrystallized from ethyl acetate/diethyl ether

出典と根拠

ORDレコード
ord-d2f6858cf02b45fb85e969b5246bb9fc
出典データセット
uspto-grants-2007_04
特許番号
US07208491B2

反応ノート

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