Hydrochloric Acid → N-Methacryloyl glycine

HRID 1632278노트

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HRID 1632278 반응식
O.[OH-].[Na+].[NH2:4][CH2:5][C:6]([OH:8])=[O:7].[N+](C1C=CC=CC=1)([O-])=O.[C:18](Cl)(=[O:22])[C:19]([CH3:21])=[CH2:20].Cl>C(#N)C>[C:18]([NH:4][CH2:5][C:6]([OH:8])=[O:7])(=[O:22])[C:19]([CH3:21])=[CH2:20]

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 750GlycineHCID 962WaterHCID 7416NitrobenzeneHCID 13528Methacryloyl chlorideHCID 14798Sodium Hydroxide2회

생성물 1

HCID 152645N-Methacryloyl glycine수율 64.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
-20 °C

실험 절차

To 400 ml of water containing 80 g (2.0 mol) of sodium hydroxide dissolved, were added 150 g (2.0 mol) of glycine and 4 ml of nitrobenzene. To the mixture, there were simultaneously added 200 ml of an aqueous solution containing 96 g (2.4 mol) of sodium hydroxide and 230 g (2.2 mol) of methacrylic chloride under cooling (at -20° C.) with stirring over a period of about 2 hours. After adding 800 ml of acetonitrile and 160 ml of concentrated hydrochloric acid, the organic layer was separated. The solvent was distilled off under a reduced pressure and the crystals thus deposited were collected by filtration and recrystallized from ethyl acetate to obtain 184 g (64.3% yield) of α-methacryloylaminoacetic acid.

후처리

  1. customthe organic layer was separated
  2. distillationThe solvent was distilled off under a reduced pressure
  3. filtrationthe crystals thus deposited were collected by filtration
  4. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-73c9e21ab43c48059e31597d3ce50d75
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04474870

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