Potassium Hydroxide → HCID 178526578、化合物

HRID 252992

反応式

HRID 252992 の反応式
[SH-:1].[C+4:2].[SH-:3].[SH-].[SH-].[N+:6]([C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]([NH:13][NH2:14])=O)([O-:8])=[O:7].[OH-].[K+]>CO>[N+:6]([C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]1[S:1][C:2]([SH:3])=[N:14][N:13]=1)([O-:8])=[O:7]

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 3781218o-NitrobenzohydrazideHCID 178420937HCID 178420937、化合物

生成物 1

HCID 178526578HCID 178526578、化合物収率 51%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Carbon bisulfide (4 ml) was added to a solution of 1.81 g (10 mmol) of 2-nitrobenzohydrazide in 8 ml of methanol. A solution of 616 mg (11 mmol) of potassium hydroxide in methanol (10 ml) was added thereto, and the mixture was stirred at room temperature for 6 hr. The precipitated crystal was collected by filtration and was dried. The dried crystal was added dropwise to 5 ml of concentrated sulfuric acid, and the mixture was stirred at room temperature for 3 hr. The reaction solution was added dropwise to 100 ml of ice water, and the resultant precipitate was collected by filtration and was dried to give 1.21 g (51%) of the title compound.

後処理

  1. filtrationThe precipitated crystal was collected by filtration
  2. customwas dried
  3. additionThe dried crystal was added dropwise to 5 ml of concentrated sulfuric acid
  4. stirringthe mixture was stirred at room temperature for 3 hr
  5. additionThe reaction solution was added dropwise to 100 ml of ice water
  6. filtrationthe resultant precipitate was collected by filtration
  7. customwas dried

出典と根拠

ORDレコード
ord-605d4926122c4a8a9888895ae597d2ec
出典データセット
uspto-grants-2011_01
特許番号
US07871982B2

関連ノート

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