Hydrazine hydrate (1:1) → HCID 23332954、化合物

HRID 224404ノート

反応式

HRID 224404 の反応式
[Cl:1][C:2]([Cl:23])([Cl:22])[CH:3]1[O:8][CH:7]([C:9](Cl)([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17](OCC)=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.O.[NH2:25][NH2:26]>C(O)C>[Cl:10][C:9]([Cl:11])=[C:7]1[C:6]2[CH:13]=[C:14]([C:17]([NH:25][NH2:26])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4][CH:3]([C:2]([Cl:23])([Cl:22])[Cl:1])[O:8]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 23332965HCID 23332965、化合物

生成物 1

HCID 23332954HCID 23332954、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of ethyl 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylate (6.4 g.), 100% hydrazine hydrate (3 ml.) and ethanol (30 ml.) was warmed on the steam bath for 30 hours. The reaction mixture was cooled, and then evaporated to dryness under reduced pressure. The oily residue was triturated with petroleum ether (b.p. 60°-80° C.) and the solid product thus obtained was crystallised from ethanol, to give 4-dichloromethylene-2-trichloromethylbenzo[1,3]dioxin-6-carbohydrazide, m.p. 182°-183° C.

後処理

  1. temperaturewas warmed on the steam bath for 30 hours
  2. temperatureThe reaction mixture was cooled
  3. customevaporated to dryness under reduced pressure
  4. customThe oily residue was triturated with petroleum ether (b.p. 60°-80° C.)
  5. customthe solid product thus obtained
  6. customwas crystallised from ethanol

出典と根拠

ORDレコード
ord-4583f278911a4bb1873c82e43ddf6246
出典データセット
uspto-grants-1980_11
特許番号
US04232032

反応ノート

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