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HCID 18536675、化合物 → HCID 18536678、化合物

HRID 412046
ノート
印刷プレビュー

反応式

HRID 412046 の反応式
[CH2:1]([O:3][CH:4]([O:12][CH2:13][CH3:14])[C:5](=O)[CH:6]([CH3:10])[C:7](=O)[CH3:8])[CH3:2].C(=O)(O)[O-].[C:19]1([NH:25][C:26]([NH2:28])=[NH2+:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH3:10][C:6]1[C:5]([CH:4]([O:12][CH2:13][CH3:14])[O:3][CH2:1][CH3:2])=[N:27][C:26]([NH:25][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:28][C:7]=1[CH3:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 18536675HCID 18536675、化合物HCID 178512436HCID 178512436、化合物

生成物 1

HCID 18536678HCID 18536678、化合物収率 114.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
75 °C

実験手順

A mixture of 44 g (purity about 50%, about 0.11 mol) of 1,1-diethoxy-3-methylpentane-2,4-dione (crude product, Example 2a) and 35 g (0.175 mol) of phenylguanidinium bicarbonate in 300 ml of ethanol was heated at 70-80° C. for about 3 hours. The reaction mixture was then concentrated and the residue was filtered, with suction, through silica gel using methyl tert-butyl ether. The solvent was evaporated. Less volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C. The residue obtained was 38 g (quantitative yield) of the title compound as a yellow oil.

後処理

  1. concentrationThe reaction mixture was then concentrated
  2. filtrationthe residue was filtered, with suction, through silica gel
  3. customThe solvent was evaporated
  4. distillationLess volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C
  5. customThe residue obtained

出典と根拠

ORDレコード
ord-f34b6f5bfc144fff828b8d7d3e3917ff
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06562833B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート