Iodine → 2-(2-Dimethylaminoethoxy)ethyl Methacrylate

HRID 582446

반응식

HRID 582446 반응식
[Mg].II.[CH3:4][N:5]([CH3:12])[CH2:6][CH2:7][O:8][CH2:9][CH2:10][OH:11].C1C2NC3C(=CC=CC=3)SC=2C=CC=1.[C:27](OC)(=[O:31])[C:28]([CH3:30])=[CH2:29]>CO>[C:27]([O:11][CH2:10][CH2:9][O:8][CH2:7][CH2:6][N:5]([CH3:12])[CH3:4])(=[O:31])[C:28]([CH3:30])=[CH2:29]

참가 물질

7

반응물 5

HCID 807IodineHCID 6658Methyl MethacrylateHCID 7108PhenothiazineHCID 743482-(2-(Dimethylamino)ethoxy)ethanolHCID 5462224Magnesium

생성물 1

HCID 158702902-(2-Dimethylaminoethoxy)ethyl Methacrylate

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A magnesium methoxide solution was prepared by dissolving magnesium metal (4 g) in anhydrous methanol (100 ml) in the presence of a small amount of iodine (approximately 0.1 g). A portion of the resulting solution (18 ml) was placed in a 250 ml reaction vessel and then 2-(2-dimethylaminoethoxy)ethanol (23.6 g) was added, followed by the addition of phenothiazine (0.1 g) and methyl methacrylate (117 g). The mixture was stirred and heated until the methanol started to distill. When all of the methanol was collected, the mixture was cooled to room temperature and the solids were filtered off. The filtrate was subjected to fractionation under reduced pressure. The excess of methyl methacrylate was separated and then pure 2-(2-dimethylaminoethoxy)ethyl methacrylate was collected at 97-102° C./4 mmHg. Yield 22.1 g.

후처리

  1. distillationto distill
  2. customWhen all of the methanol was collected
  3. filtrationthe solids were filtered off
  4. customThe excess of methyl methacrylate was separated
  5. custompure 2-(2-dimethylaminoethoxy)ethyl methacrylate was collected at 97-102° C./4 mmHg

출처 및 근거

ORD 기록
ord-d1ed5f33d9364e8cb4ab1b7b339ae5e7
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925253

연결된 노트

불러오는 중…