Toluene → HCID 19738525、化合物

HRID 1646025ノート

反応式

HRID 1646025 の反応式
[H-].[Na+].C1(C)C=CC=CC=1.[CH3:10][O:11][CH:12]([O:20][CH3:21])[CH2:13][NH:14][C:15](=[O:19])[O:16][CH2:17][CH3:18].Cl[CH2:23][C:24]([CH2:26][F:27])=[CH2:25]>O>[F:27][CH2:26][C:24](=[CH2:23])[CH2:25][N:14]([CH2:13][CH:12]([O:11][CH3:10])[O:20][CH3:21])[C:15](=[O:19])[O:16][CH2:17][CH3:18]

参加物

6

反応物 4

HCID 1140TolueneHCID 24758Sodium hydrideHCID 10921057Ethyl 2,2-dimethoxyethylcarbamateHCID 140720532-(Chloromethyl)-3-fluoroprop-1-ene

生成物 1

HCID 19738525HCID 19738525、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

8 g (0.26 mol) of sodium hydride (80% pure) are initially introduced into 200 ml of toluene and 35.8 g (0.2 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate are added dropwise at 90° C. The mixture is then stirred for one hour at 90° C. and 32.6 g (0.3 mol) of 1-chloro-2-fluoromethylprop-2-ene are then added dropwise. The mixture is stirred overnight at 90° C., salts are dissolved in water, and the aqueous phase is separated off and extracted with toluene. The organic phases are dried over potassium carbonate and concentrated, and the residue is distilled.

後処理

  1. additionare added dropwise at 90° C
  2. stirringThe mixture is stirred overnight at 90° C.
  3. customthe aqueous phase is separated off
  4. extractionextracted with toluene
  5. dry with materialThe organic phases are dried over potassium carbonate
  6. concentrationconcentrated
  7. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-bbeb7ecf03b645829589cd0f6e061a11
出典データセット
uspto-grants-1993_01
特許番号
US05177210

反応ノート

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