Hydrochloric Acid → 4-Cyano-4'-trifluoromethylbutyrophenone O-(2-aminoethyl) oxime hydrochloride

HRID 2083394노트

반응식

HRID 2083394 반응식
[C:1]([CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=1)=O)#[N:2].[ClH:18].Cl.[NH2:20][O:21][CH2:22][CH2:23][NH2:24].N1C=CC=CC=1.Cl>C(O)C>[ClH:18].[NH2:24][CH2:23][CH2:22][O:21][N:20]=[C:6]([C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=1)[CH2:5][CH2:4][CH2:3][C:1]#[N:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 143623262-(O-aminooxy)ethylamine dihydrochlorideHCID 203585325-Oxo-5-(4-trifluoromethylphenyl)valeronitrile

생성물 1

HCID 867356254-Cyano-4'-trifluoromethylbutyrophenone O-(2-aminoethyl) oxime hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

5.6 Mmol (1.35 g) of 4-cyano-4'-trifluoromethylbutyrophenone, 5.6 mmol (0.84 g) of 2 aminooxyethylamine dihydrochloride and 0.8 ml of pyridine were refluxed in 20 ml of absolute ethanol for 2.5 hours. The processing was equal to that of example 1. The resulting free base was dissolved in absolute ethanol and an equivalent quantity of 2N alcoholic hydrochloric acid was added. The ethanol was then removed in vacuo and the residue was crystallized twice from ethanol/ether (1:5). The melting point of the resulting title compound was 136°-136.5° C.

후처리

  1. customThe ethanol was then removed in vacuo
  2. customthe residue was crystallized twice from ethanol/ether (1:5)
  3. customwas 136°-136.5° C.

출처 및 근거

ORD 기록
ord-cd98fd0404eb4f61809f5482a0c88104
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04085225

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