Sodium Bicarbonate → HCID 10362721、化合物

HRID 1271856ノート

反応式

HRID 1271856 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][O:29][CH2:30][CH2:31][O:32][CH3:33])=[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][O:29][CH2:30][CH2:31][O:32][CH3:33])=[CH:25][C:19]=2[CH:18]=1)=[O:16]

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 86593875HCID 86593875、化合物

生成物 1

HCID 10362721HCID 10362721、化合物収率 62.8%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 80 mg (0.164 mmol) of [2-({5-[2-(2-Methoxy-ethoxy)-ethoxy]-benzo[b]thiophene-2-carbonyl}-amino)-phenyl]-carbamic acid tert-butyl ester (28) in 1.0 ml trifluoroacetic acid was stirred for 45 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/heptane to yield 40 mg (0.103 mmol) of the desired product (27) as white crystals, mp. 167–168° C.

後処理

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

出典と根拠

ORDレコード
ord-dca74ae1eaf148c1ae454ec44ad3f05b
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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