Formaldehyde → HCID 19994807, 화합물

HRID 1110380노트

반응식

HRID 1110380 반응식
Cl.[Cl:2][CH2:3][CH2:4][CH:5]([CH3:22])[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14]C2C=CC=CC=2)[CH2:10][CH:9]1[CH3:21])=[O:7].C=O.[H][H]>[Pd].CO>[ClH:2].[Cl:2][CH2:3][CH2:4][CH:5]([CH3:22])[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH:9]1[CH3:21])=[O:7]

참가 물질

6

반응물 3

HCID 712FormaldehydeHCID 19994828HCID 19994828, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 19994807HCID 19994807, 화합물수율 72.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 16 parts of 1-(4-chloro-2-methyl-1-oxobutyl)-2-methyl-4-(phenylmethyl)piperazine monohydrochloride, 200 parts of methanol and 7 parts of a formaldehyde solution 40% was hydrogenated at normal pressure and at 60° C. with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the hydrochloride salt in 2-propanol and 2,2'-oxybispropane, yielding 9 parts (72.6%) of 1(-4-chloro-2-methyl-1-oxobutyl)-2,4-dimethylpiperazine monohydrochloride (int. 26).

후처리

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was purified by column chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-9706057aabe14bf3a2f709efe1337d18
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04975439

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