Ammonia → Flunamine

HRID 2072215

반응식

HRID 2072215 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[O:9][CH2:10][CH2:11]Cl)=[CH:4][CH:3]=1.[NH3:20].O>CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[O:9][CH2:10][CH2:11][NH2:20])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 962WaterHCID 107793021-[Bis(4-fluorophenyl)methoxy]-2-chloroethane

생성물 1

HCID 39658Flunamine수율 58.5%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
135 °C

실험 절차

A mixture of 28.2 g (0.1 mole) of 2-[bis(p-fluorophenyl)methoxy]ethyl chloride and 17 g (1 mole) of ammonia in 187.5 ml of methanol is shaken in an autoclave for a period of 6 hours at 135° C. The reaction mixture is poured into water and extracted with diethyl ether. The extract is acidified with 2N hydrochloric acid. The acid aqueous layer is separated off, made alkaline with 2N sodium hydroxide and extracted with diethyl ether. The extract is dried over potassium carbonate and the ether is distilled off. The residue is distilled, yielding 15.4 g of 2-[bis(p-fluorophenyl)-methoxy]ethylamine, boiling point 130° C./0.2 mm.Hg. The base is dissolved in diethyl ether and an ethereal solution of maleic acid is added. The precipitate is filtered off and crystallised from a mixture of ethanol and diethyl ether. 2-[Bis(p-fluorophenyl)methoxy]ethylamine hydrogen maleate is obtained. Its melting point is 126°-127° C.

후처리

  1. extractionextracted with diethyl ether
  2. customThe acid aqueous layer is separated off
  3. extractionextracted with diethyl ether
  4. dry with materialThe extract is dried over potassium carbonate
  5. distillationthe ether is distilled off
  6. distillationThe residue is distilled

출처 및 근거

ORD 기록
ord-289e1190599740a286f1866ce4d61956
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04049825

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