Potassium Hydroxide → HCID 23050230、化合物

HRID 978739ノート

反応式

HRID 978739 の反応式
Cl.[NH2:2][OH:3].[OH-].[K+].C([O:8][C:9]([C:11]1[S:15][C:14]2[CH:16]=[C:17]([O:22][CH3:23])[C:18]([O:20][CH3:21])=[CH:19][C:13]=2[CH:12]=1)=O)C>C(O)C>[OH:3][NH:2][C:9]([C:11]1[S:15][C:14]2[CH:16]=[C:17]([O:22][CH3:23])[C:18]([O:20][CH3:21])=[CH:19][C:13]=2[CH:12]=1)=[O:8]

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 45104330Ethyl 5,6-dimethoxybenzo[b]thiophene-2-carboxylate

生成物 1

HCID 23050230HCID 23050230、化合物収率 87.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒3 回

実験手順

Hydroxylamine hydrochloride (5.3 g) was dissolved in warm ethanol (100 ml). The solution was stirred under an atmosphere of nitrogen and treated with a warm solution of potassium hydroxide (6.4 g) in ethanol (50 ml). After 10 min. a solution of 5,6-dimethoxy-benzo[b]thiophene-2-carboxylic acid ethyl ester (10 g) in ethanol (250 ml) was added and the resultant mixture was allowed to stand at room temperature for 72 hours. The resultant suspension was filtered to remove the precipitated potassium chloride and the filtrate was evaporated to dryness. The resultant yellow residue was dissolved in water (250 ml), filtered and the filtrate was acidified with 5M hydrochloric acid. The precipitated product was filtered and dried at 65° C. under vacuum to give N-hydroxy-5,6-dimethoxy-benzo[b]thiophene-2-carboxamide (8.3 g). A portion crystallised from acetone had a melting point: 179°-180° C.

後処理

  1. filtrationThe resultant suspension was filtered
  2. customto remove the precipitated potassium chloride
  3. customthe filtrate was evaporated to dryness
  4. dissolutionThe resultant yellow residue was dissolved in water (250 ml)
  5. filtrationfiltered
  6. filtrationThe precipitated product was filtered
  7. customdried at 65° C. under vacuum

出典と根拠

ORDレコード
ord-9fdc74da5454476687410bd57c34be09
出典データセット
uspto-grants-1987_05
特許番号
US04665206

反応ノート

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