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

HRID 2107620노트

반응식

HRID 2107620 반응식
[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

참가 물질

7

반응물 2

HCID 27367824-Methoxythiophene-3-carbohydrazideHCID 23668193Sodium Nitrite

생성물 1

HCID 230461504-Methoxy-3-thiophenecarbonyl azide

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매HCID 962Water용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cb08a73f1c2448f9a9ae105d013b4371
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04935431

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