2,5-二羟基甲苯 → 2-[N',N'-Bis(2-hydroxyethyl)ureido]ethyl Methacrylate

HRID 4694

反应方程式

HRID 4694 反应方程式
[NH:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].CC1C=C(O)C=CC=1O.[C:17]([O:22][CH2:23][CH2:24][N:25]=[C:26]=[O:27])(=[O:21])[C:18]([CH3:20])=[CH2:19]>C1(C)C=CC=CC=1>[C:17]([O:22][CH2:23][CH2:24][NH:25][C:26]([N:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4])=[O:27])(=[O:21])[C:18]([CH3:20])=[CH2:19]

参与物

5

反应物 3

HCID 72532,5-二羟基甲苯HCID 8113二乙醇胺HCID 35409甲基丙烯酸异氰基乙酯

产物 1

HCID 191024562-[N',N'-Bis(2-hydroxyethyl)ureido]ethyl Methacrylate

试剂、催化剂与溶剂 1

HCID 1140甲苯溶剂

实验过程

A one liter flask, under a N2 blanket, was charged with 105 gm of diethanolamine (1 mole) and 20 mg of methylhydroquinone. One molar of 2-isocyanatoethyl methacrylate (IEM) containing 2 ml of DBTDL (2% solution in toluene) was dropped slowly in the flask with moderate stirring over a period of 105 minutes, while the temperature was maintained at 20° to 25° C. with an ice-bath. The resulting viscous solution was stirred for an additional 60 minutes at 20° C. and then discharged. The product showed no NCO absorption in the IR spectrum and the NMR spectrum was consistent with the proposed structure. Gas chromatography also indicated the purity of the product to be greater than 95%. Additional inhibitor was added (to a total of 250 ppm) and the diol was stored in a freezer.

后处理

  1. additionwas dropped slowly in the flask
  2. temperaturewas maintained at 20° to 25° C. with an ice-bath
  3. stirringThe resulting viscous solution was stirred for an additional 60 minutes at 20° C.
  4. customno NCO absorption in the IR spectrum
  5. additionAdditional inhibitor was added (to a total of 250 ppm) and the diol

来源与证据

ORD记录
ord-90f1210b5010478582a8b8c2ecc022ac
来源数据集
uspto-grants-1988_02
专利号
US04727126

关联笔记

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