Hydrazine hydrate (1:1) → HCID 18430681、化合物

HRID 378831

反応式

HRID 378831 の反応式
[C:1]1([C:7]2[C:8](O[C:11](=[O:13])[CH:12]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.O.O.C([O-])(=O)C.[Na+].O.[NH2:23][NH2:24]>C(O)(=O)C>[C:1]1([C:7]2[C:8](=[O:9])[N:23]=[N:24][C:11](=[O:13])[CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 24654Hydrazine hydrate (1:1)HCID 99174Phenylmaleic anhydrideHCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 18430681HCID 18430681、化合物収率 33.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Phenylmaleic anhydride (20 g, 115 mmol), sodium acetate trihydrate (1875 g, 138 mmol), hydrazine monohydrate (6.68 ml, 133 mmol) and 40% aqueous acetic acid (400 ml) were heated at reflux for 15 h then allowed to cool. The reaction mixture was left to cool in the fridge for 1 h. The solid produced was filtered and washed with water and diethyl ether before drying in a vacuum oven at 40° C. to give the required product (7.26 g). 1H NMR (250 MHz, DMSO) δ 3.43 (2H, broad peak), 7.17 (1H, s), 7.44 (3H, m), 7.81 (2H, m); MS (ES+) m/e 189 [MH+].

後処理

  1. temperatureat reflux for 15 h
  2. temperatureto cool
  3. waitThe reaction mixture was left
  4. temperatureto cool in the fridge for 1 h
  5. customThe solid produced
  6. filtrationwas filtered
  7. washwashed with water and diethyl ether
  8. custombefore drying in a vacuum oven at 40° C.

出典と根拠

ORDレコード
ord-0b3c74bd81ff4dd9a780a64a0ba0942c
出典データセット
uspto-grants-2001_10
特許番号
US06297235B1

関連ノート

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