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Ammonia → HCID 22666426、化合物

HRID 1007889
ノート
印刷プレビュー

反応式

HRID 1007889 の反応式
[CH2:1]([N:3]([CH2:21][CH3:22])[CH2:4][CH2:5][O:6][CH2:7][CH2:8][C:9]1[CH:20]=[CH:19][C:12]2[S:13][C:14]([C:16](O)=[O:17])=[CH:15][C:11]=2[CH:10]=1)[CH3:2].[NH3:23].C(OCC)(=O)C>O1CCCC1>[CH2:1]([N:3]([CH2:21][CH3:22])[CH2:4][CH2:5][O:6][CH2:7][CH2:8][C:9]1[CH:20]=[CH:19][C:12]2[S:13][C:14]([C:16]([NH2:23])=[O:17])=[CH:15][C:11]=2[CH:10]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 222AmmoniaHCID 8857Ethyl AcetateHCID 22666517HCID 22666517、化合物

生成物 1

HCID 22666426HCID 22666426、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In 30 mL of tetrahydrofuran is dissolved 2.18 g of 5-{2-[2-(diethylamino)ethoxy]ethyl}benzo[b]-thiophene-2-carboxylic acid, to which is added 1.98 g of N,N′-carbonyldiimidazole. The resulting mixture is stirred at ambient temperature for one hour. Then, 50 mL of 25% aqueous ammonia is added to the mixture and the resulting mixture is stirred at ambient temperature for one hour. Ethyl acetate is added to the mixture, the organic layer is separated, washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, the solvent is distilled off under reduced pressure, and the residue is purified by column chromatography (eluent:chloroform:methanol to chloroform:methanol:ammonia=5:1 to 100:10:1). Thus, 2.00 g of 5-{2-[2-(diethylamino)ethoxy]ethyl}benzo[b]-thiophene-2-carboxamide is obtained as a colorless crystalline product.

後処理

  1. stirringthe resulting mixture is stirred at ambient temperature for one hour
  2. customthe organic layer is separated
  3. washwashed with water and saturated aqueous solution of sodium chloride successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customthe residue is purified by column chromatography (eluent:chloroform:methanol to chloroform:methanol:ammonia=5:1 to 100:10:1)

出典と根拠

ORDレコード
ord-4b60e3a85a694ae89a22d924c0b08bdc
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06797726B1

反応ノート

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