Diethyl Carbonate → HCID 10922274、化合物

HRID 1087756

反応式

HRID 1087756 の反応式
[CH2:1]([OH:14])[CH:2]([OH:13])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[C:15](=O)(OCC)[O:16]CC>[H-].[Na+].C1C=CC=CC=1>[CH2:3]([CH:2]1[CH2:1][O:14][C:15](=[O:16])[O:13]1)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

5

反応物 2

HCID 7766Diethyl CarbonateHCID 928661,2-Dodecanediol

生成物 1

HCID 10922274HCID 10922274、化合物収率 108.1%

試薬・触媒・溶媒 2

HCID 24758Sodium hydride触媒HCID 241Benzene溶媒

実験手順

A 125 ml round bottom flask equipped with a Dean-Stark trap was charged with 10 g of 1,2-dodecanediol, 7.1 g of diethyl carbonate and 50 ml of benzene. The solution was stirred until homogeneous and then 50 mg of 60% NaH was added. The reaction mixture was refluxed for 6 hours and then concentrated to afford 12.2 g of oil. This was taken up in 100 ml of pet. ether and allowed to crystallize in freezer whereupon 1.1 g of starting diol was recovered. Concentration of the filtrate gave 9.53 g (89.66%) of a colorless oil.

後処理

  1. customA 125 ml round bottom flask equipped with a Dean-Stark trap
  2. additionwas added
  3. temperatureThe reaction mixture was refluxed for 6 hours
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-de66ac2a3c5d417aa9ae689bf65be204
出典データセット
uspto-grants-1990_10
特許番号
US04960771

関連ノート

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