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

Glycerol → 1,3-Dioxolane-4-methanol, 2-ethyl-2-methyl-

HRID 431304
ノート
印刷プレビュー

反応式

HRID 431304 の反応式
[CH2:1]([C:3]([CH3:5])=[O:4])[CH3:2].[OH:6][CH2:7][CH:8]([CH2:10]O)[OH:9].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>CCCCCC>[CH3:5][C:3]1([CH2:1][CH3:2])[O:9][CH:8]([CH2:7][OH:6])[CH2:10][O:4]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 753GlycerolHCID 6569Methyl Ethyl KetoneHCID 10340Sodium CarbonateHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 118049031,3-Dioxolane-4-methanol, 2-ethyl-2-methyl-

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

反応条件

温度
60 °C

実験手順

In a reaction vessel having a capacity of 3 L and equipped with a thermometer, a reflux condenser, a Dean-Stark trap, a calcium chloride tube and a stirrer, methyl ethyl ketone (400 g, 5,547 mol), glycerin (561.91 g, 6.102 mol), paratoluene-sulfonic acid monohydrate (21.10 g, 0.1109 mol) and hexane (400 mL) were charged. The contents were heated under stirring and a reaction was conducted at 67 to 74° C. for 30 hours to distill off a calculated amount of water. After completion of the reaction, the reaction mixture was cooled to 60° C., followed by the addition of sodium carbonate (23.51 g, 0.2218 mol) for neutralization. After the resulting mixture was stirred at 60° C. for 30 minutes, the temperature was gradually raised up to 120° C. to recover hexane (400 mL). Filtration was then conducted to obtain the titled product in a crude form (894.74 g). Using a Biglew tube (20 cm×1.5 cm in diameter), distillation was conducted under reduced pressure to obtain the titled compound (725.14 g, yield: 89.4%). By a gas chromatographic analysis, the purity of the compound was found to be 99.1 wt. %. b.p. 101 to 104° C./17 mmHg.

後処理

  1. customIn a reaction vessel having
  2. customa capacity of 3 L and equipped with a thermometer, a reflux condenser
  3. temperatureThe contents were heated
  4. distillationto distill off a calculated amount of water
  5. customAfter completion of the reaction
  6. stirringAfter the resulting mixture was stirred at 60° C. for 30 minutes
  7. temperaturethe temperature was gradually raised up to 120° C.
  8. customto recover hexane (400 mL)
  9. filtrationFiltration

出典と根拠

ORDレコード
ord-7bcae3e6bd9b402eb284faa48332f3f4
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06657089B1

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