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Ethanol → HCID 14274201、化合物

HRID 1032003
ノート
印刷プレビュー

反応式

HRID 1032003 の反応式
[CH3:1][S:2]([NH:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH:8]=[CH:9][CH:10]=[C:11]2[OH:16])(=[O:4])=[O:3].C(O)C.[N:20]([O-])=[O:21].[Na+]>O.[Cl-].[Zn+2].[Cl-]>[N:20]([C:10]1[CH:9]=[CH:8][C:7]2[C:12](=[CH:13][CH:14]=[CH:15][C:6]=2[NH:5][S:2]([CH3:1])(=[O:4])=[O:3])[C:11]=1[OH:16])=[O:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 702EthanolHCID 104704Methanesulfonamide, N-(5-hydroxy-1-naphthalenyl)-HCID 23668193Sodium Nitrite

生成物 1

HCID 14274201HCID 14274201、化合物

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 962Water溶媒2 回

反応条件

温度
50 °C

実験手順

A mixture comprising 119 g of 5-methanesulfonylamino-1-naphthol, 100 g of zinc chloride and 500 ml of ethanol was heated at 50° C., and then a solution of 35 g of sodium nitrite as dissolved in 70 ml of water was added dropwise thereto at 50° to 65° C. After being heated and stirred at 60° to 65° C. for 2 hours, the resulting solution was cooled with water to room temperature, and reddish brown crystals formed were taken out by filtration and washed with ethanol. The crystals were added to 200 ml of concentrated hydrochloric acid and stirred for 1 hour at room temperature, and then 200 ml of water was added thereto. Yellowish brown crystals (2-nitroso-5-methanesulfonylamino-1-naphthol) formed were taken out by filtration, washed with water and dried. Yield: 90 g.

後処理

  1. additionwas added dropwise
  2. customat 50° to 65° C
  3. temperatureAfter being heated
  4. customformed
  5. filtrationwere taken out by filtration
  6. washwashed with ethanol
  7. additionThe crystals were added to 200 ml of concentrated hydrochloric acid
  8. stirringstirred for 1 hour at room temperature
  9. addition200 ml of water was added

出典と根拠

ORDレコード
ord-9abec76542314cb5849ae40ff6f0558d
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04956456

反応ノート

読み込み中…

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