Formic Acid → HCID 13714730、化合物

HRID 65095ノート

反応式

HRID 65095 の反応式
[CH:1]([C:4]([C:24]1[CH:29]=[C:28]([O:30][CH3:31])[C:27]([O:32][CH3:33])=[C:26]([O:34][CH3:35])[CH:25]=1)([CH2:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N+:21]([O-:23])=[O:22])[C:5]#[N:6])([CH3:3])[CH3:2].C=O.[CH:38](O)=O.C(=O)([O-])[O-].[K+].[K+]>O>[CH:1]([C:4]([C:24]1[CH:29]=[C:28]([O:30][CH3:31])[C:27]([O:32][CH3:33])=[C:26]([O:34][CH3:35])[CH:25]=1)([CH2:7][CH2:8][CH2:9][N:10]([CH2:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N+:21]([O-:23])=[O:22])[CH3:38])[C:5]#[N:6])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 11430Potassium CarbonateHCID 13714726HCID 13714726、化合物

生成物 1

HCID 13714730HCID 13714730、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2.58 g of alpha-isopropyl-alpha-[3-[N-[3-(2-nitrophenoxy)propyl]amino]propyl]-3,4,5-trimethoxyphenylacetonitrile, 4.35 ml of 37% of formalin, and 4.35 ml of 90% formic acid was stirred for 1 hour at 90° 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 1% methanol-chloroform as an eluent to give 1.43 g of the desired compound as a 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 using 1% methanol-chloroform as an eluent

出典と根拠

ORDレコード
ord-5983842ea241493c865f5382b3a6641a
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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