Triethylamine → 4-Methoxybenzyl(2-methoxyethyl)carbamoyl chloride

HRID 2212962ノート

反応式

HRID 2212962 の反応式
ClC([O:4][C:5]([Cl:8])(Cl)Cl)=O.[CH3:9][O:10][C:11]1[CH:22]=[CH:21][C:14]([CH2:15][NH:16][CH2:17][CH2:18][O:19][CH3:20])=[CH:13][CH:12]=1.C(N(CC)CC)C>ClCCl>[CH3:9][O:10][C:11]1[CH:22]=[CH:21][C:14]([CH2:15][N:16]([CH2:17][CH2:18][O:19][CH3:20])[C:5]([Cl:8])=[O:4])=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10426DiphosgeneHCID 32858732-methoxy-N-(4-methoxybenzyl)ethanamine

生成物 1

HCID 219560334-Methoxybenzyl(2-methoxyethyl)carbamoyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.51 g (0.31 ml, 2.56 mmol) of trichloromethyl chloroformate (“diphosgene”) are dissolved in 15 ml of dichloromethane, and 1.00 g (5.12 mmol) of 4-methoxybenzyl(2-methoxyethyl)amine and 0.78 g (7.68 mmol) of triethylamine are slowly added. After stirring at room temperature overnight, the mixture is poured into ice-water and extracted three times with dichloromethane, and the organic phase is dried over magnesium sulfate and concentrated to dryness in a rotary evaporator. The crude product is employed without workup directly in the next stage.

後処理

  1. extractionextracted three times with dichloromethane
  2. dry with materialthe organic phase is dried over magnesium sulfate
  3. concentrationconcentrated to dryness in a rotary evaporator

出典と根拠

ORDレコード
ord-18912abb5e604afb8af2d2a4c934ad19
出典データセット
uspto-grants-2006_09
特許番号
US07105523B2

反応ノート

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