Hydrazine hydrate (1:1) → HCID 23332954, 화합물

HRID 224404노트

반응식

HRID 224404 반응식
[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

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 23332965HCID 23332965, 화합물

생성물 1

HCID 23332954HCID 23332954, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4583f278911a4bb1873c82e43ddf6246
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232032

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