Potassium Carbonate → HCID 20041122、化合物

HRID 1762556ノート

反応式

HRID 1762556 の反応式
[OH:1][CH:2]([CH2:16][OH:17])[CH2:3][N:4]1[C:12]2[C:11](=[O:13])[NH:10][C:9](=[O:14])[N:8]([CH3:15])[C:7]=2[N:6]=[CH:5]1.Cl[CH2:19][CH2:20][CH2:21][CH2:22][C:23]([OH:26])([CH3:25])[CH3:24].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[OH:1][CH:2]([CH2:16][OH:17])[CH2:3][N:4]1[C:12]2[C:11](=[O:13])[N:10]([CH2:19][CH2:20][CH2:21][CH2:22][C:23]([OH:26])([CH3:25])[CH3:24])[C:9](=[O:14])[N:8]([CH3:15])[C:7]=2[N:6]=[CH:5]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 3616685AC1MUDJSHCID 137476791-Chloro-5-hydroxy-5-methylhexane

生成物 1

HCID 20041122HCID 20041122、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

A mixture of 18 g (0.075 mol) of the xanthine compound from stage (a), 12.5 g (0.083mol) of 1-chloro-5-hydroxy-5-methylhexane (Example 1a) and 11.5 g (0.083 mol) of potassium carbonate in 500 ml of dimethylformamide is stirred for 18 hours at 110° C., after which the hot mixture is filtered and the filtrate is concentrated in vacuo. The oily crude product, which gradually crystallizes through, can advantageously be purified by filtration over a silica gel column using a chloroform/methanol (10:1) solvent mixture, followed by a final recrystallization from ethyl acetate with the addition of petroleum ether, at the boil.

後処理

  1. filtrationafter which the hot mixture is filtered
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe oily crude product, which gradually crystallizes through,
  4. filtrationcan advantageously be purified by filtration over a silica gel column
  5. customrecrystallization from ethyl acetate
  6. additionwith the addition of petroleum ether

出典と根拠

ORDレコード
ord-4c5596507ba14ffba2e2f104168b3061
出典データセット
uspto-grants-1989_05
特許番号
US04833146

反応ノート

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