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Triethylamine → HCID 15055173、化合物

HRID 1463382
ノート
印刷プレビュー

反応式

HRID 1463382 の反応式
[C:1](Cl)(=[O:5])[C:2]([CH3:4])=[CH2:3].[OH:7][CH2:8][CH2:9][CH2:10][NH:11][C:12](=[O:14])[CH3:13].C(N(CC)CC)C>C(C1C=C(C)C=C(C(C)(C)C)C=1O)(C)(C)C.C(Cl)Cl>[C:1]([O:7][CH2:8][CH2:9][CH2:10][NH:11][C:12](=[O:14])[CH3:13])(=[O:5])[C:2]([CH3:4])=[CH2:3]
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 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 2781177N-(3-hydroxypropyl)acetamide

生成物 1

HCID 15055173HCID 15055173、化合物収率 53.4%

試薬・触媒・溶媒 2

HCID 314042,6-Di-tert-butyl-4-methylphenol触媒HCID 6344Dichloromethane溶媒

反応条件

温度
-72 °C

実験手順

184.0 g (1.76 mol) of methacryloyl chloride were added dropwise in the course of 2 hours to an initial mixture, cooled to -72° C., consisting of 206.2 g (1.76 mol) of N-(3-hydroxypropyl)-acetamide, 750 ml of methylene chloride, 228 g (2.25 mol) of triethylamine and 250 mg of 2,6-di-tert.butyl-4-methylphenol. The mixture was stirred for a further 2 hours at -52° C. and the precipitated pale precipitate was then filtered off with suction at 0° C. The filtrate was subjected to aqueous work-up and the product was dried and, after concentrating on a rotary evaporator, distilled first at 100° C., and then the residue at 130° C. (in each case 0.1 mm Hg). 174.1 g (53% of theory) of 3- acetamidopropyl methacrylate were obtained in the form of a colorless oil.

後処理

  1. filtrationthe precipitated pale precipitate was then filtered off with suction at 0° C
  2. customthe product was dried
  3. concentrationafter concentrating on a rotary evaporator
  4. distillationdistilled first at 100° C.
  5. customat 130° C.

出典と根拠

ORDレコード
ord-dbee653892a94d3981ad2cabc6b45da6
出典データセット
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05300537

反応ノート

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