ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 2-Hydroxymethyl-8-methoxy-1,4-benzodioxan

HRID 2259919
ノート
印刷プレビュー

反応式

HRID 2259919 の反応式
[OH:1][C:2]1[C:7]2[O:8][CH:9]([CH2:12][OH:13])[CH2:10][O:11][C:6]=2[CH:5]=[CH:4][CH:3]=1.[C:14](=O)([O-])[O-].[K+].[K+].CI.O>CN(C)C=O>[OH:13][CH2:12][CH:9]1[O:8][C:7]2[C:2]([O:1][CH3:14])=[CH:3][CH:4]=[CH:5][C:6]=2[O:11][CH2:10]1
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

6

反応物 4

HCID 962WaterHCID 6328Methyl iodide3 回HCID 11430Potassium Carbonate2 回HCID 143491888-Hydroxy-1,4-benzodioxan-2-ylmethanol

生成物 1

HCID 104881082-Hydroxymethyl-8-methoxy-1,4-benzodioxan収率 90%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

反応条件

温度
45 °C

実験手順

A mixture of 5.52 g of 8-hydroxy-2-hydroxymethyl-1,4-benzodioxan (prepared as described in EP 210581), 4.2 g of anhydrous potassium carbonate and 2.06 ml of methyl iodide in 75 ml of anhydrous dimethylformamide was stirred at 45° C. for 8 hours. Methyl iodide (1 ml) was added to the mixture and stirring continued at the same temperature. After 8 hours, 1 ml of methyl iodide and 2.1 g of potassium carbonate were further added, and the reaction mixture was stirred at 45° C. for 6 hours. Thereafter, the mixture was cooled to room temperature, poured into water and extracted with ethyl acetate. The organic layer was washed with 6N aqueous sodium hydroxide solution, water, then dried on sodium sulfate. Evaporation of the organic layer to dryness in vacuo afforded 5.35 g of 2-hydroxymethyl-8-methoxy- 1,4-benzodioxan, which was used in the next step without further purification.

後処理

  1. stirringstirring
  2. waitAfter 8 hours
  3. stirringthe reaction mixture was stirred at 45° C. for 6 hours
  4. temperatureThereafter, the mixture was cooled to room temperature
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with 6N aqueous sodium hydroxide solution, water
  7. customdried on sodium sulfate
  8. customEvaporation of the organic layer to dryness in vacuo

出典と根拠

ORDレコード
ord-8f8a3091a7a3426ba9191b01613e1399
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05474994

反応ノート

読み込み中…

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