Formic Acid → Alpha-isopropyl-alpha-[3-[N-[2-(2-methoxyphenoxy)ethyl]-N-methylamino]propyl]-3,4-dimethoxyphenylacetonitrile

HRID 65091ノート

反応式

HRID 65091 の反応式
[CH:1]([C:4]([C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1)([CH2:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[O:20][CH3:21])[C:5]#[N:6])([CH3:3])[CH3:2].C=O.[CH:34](O)=O.C(=O)([O-])[O-].[K+].[K+]>O>[CH:1]([C:4]([C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1)([CH2:7][CH2:8][CH2:9][N:10]([CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[O:20][CH3:21])[CH3:34])[C:5]#[N:6])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 11430Potassium CarbonateHCID 13714717HCID 13714717、化合物

生成物 1

HCID 13714723Alpha-isopropyl-alpha-[3-[N-[2-(2-methoxyphenoxy)ethyl]-N-methylamino]propyl]-3,4-dimethoxyphenylacetonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

A mixture of 2.35 g of alpha-isopropyl-alpha-[3-[N-[2-(2-methoxyphenoxy)ethyl]amino]propyl]-3,4-dimethoxyphenylacetonitrile, 8 ml of 37% formalin, and 16 ml of 90% formic acid was stirred for 1 hour at 110° C. After cooling, to the mixture were added water and potassium carbonate to make it alkaline. The solution was extracted with chloroform and the extract was washed with water, dried, and evaporated. The residue was chromatographed on silica gel using chloroform as an eluent to give 1.30 g of the desired compound as a pale yellow oil.

後処理

  1. temperatureAfter cooling, to the mixture
  2. extractionThe solution was extracted with chloroform
  3. washthe extract was washed with water
  4. customdried
  5. customevaporated
  6. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-cc569b6f1a1549a99702b4408dea148b
出典データセット
uspto-grants-1986_09
特許番号
US04612329

反応ノート

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