Formaldehyde → HCID 19994807、化合物

HRID 1110380ノート

反応式

HRID 1110380 の反応式
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]

参加物

6

反応物 3

HCID 712FormaldehydeHCID 19994828HCID 19994828、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 19994807HCID 19994807、化合物収率 72.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9706057aabe14bf3a2f709efe1337d18
出典データセット
uspto-grants-1990_12
特許番号
US04975439

反応ノート

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