4-Methoxythiophene-3-carbohydrazide → 4-Methoxy-3-thiophenecarbonyl azide

HRID 2107620ノート

反応式

HRID 2107620 の反応式
[CH3:1][O:2][C:3]1[C:4]([C:8]([NH:10][NH2:11])=[O:9])=[CH:5][S:6][CH:7]=1.[N:12]([O-])=O.[Na+]>Cl.C(O)(=O)C.C(Cl)(Cl)Cl.O>[CH3:1][O:2][C:3]1[C:4]([C:8]([N:10]=[N+:11]=[N-:12])=[O:9])=[CH:5][S:6][CH:7]=1

参加物

7

反応物 2

HCID 27367824-Methoxythiophene-3-carbohydrazideHCID 23668193Sodium Nitrite

生成物 1

HCID 230461504-Methoxy-3-thiophenecarbonyl azide

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

4-Methoxy-3-thiophenecarboxylic acid hydrazide (20 g, 0.116 mol) in 3N hydrochloric acid (200 ml), acetic acid (200 ml) and chloroform (300 ml) was cooled to 0°. Sodium nitrite (8 g, 0.116 mol) in water (25 ml) was added dropwise whilst maintaining the temperature at 0°. On completion of the addition the reaction mixture was allowed to warm up to room temperature. The organic layer was separated, washed with sodium bicarbonate solution (3 times), dried over sodium sulphate and the solvent evaporated without heat to give the title compound as a buff-coloured solid, 21.2 g.

後処理

  1. temperaturewhilst maintaining the temperature at 0°
  2. additionOn completion of the addition the reaction mixture
  3. customThe organic layer was separated
  4. washwashed with sodium bicarbonate solution (3 times)
  5. dry with materialdried over sodium sulphate
  6. customthe solvent evaporated
  7. temperaturewithout heat

出典と根拠

ORDレコード
ord-cb08a73f1c2448f9a9ae105d013b4371
出典データセット
uspto-grants-1990_06
特許番号
US04935431

反応ノート

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