Potassium Carbonate → Diacetone acrylamide oxime

HRID 1703051노트

반응식

HRID 1703051 반응식
[C:1]([NH2:5])(=O)[CH:2]=[CH2:3].[CH3:6][C:7]([CH3:9])=[O:8].[CH3:10][C:11]([CH3:13])=[O:12].Cl.[NH2:15][OH:16].C(=O)([O-])[O-].[K+].[K+]>O>[C:1](=[N:15][OH:16])([NH2:5])[CH:2]=[CH2:3].[CH3:6][C:7]([CH3:9])=[O:8].[CH3:10][C:11]([CH3:13])=[O:12]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 215849214-Acrylamido-4-methyl-2-pentanone

생성물 1

HCID 86738575Diacetone acrylamide oxime수율 82%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution of 408 g. (2.4 moles) of diacetone acrylamide ##STR12## and 200 g. (2.88 moles; 20% molar excess) of hydroxylamine hydrochloride in 1.5 l. of distilled water was added a solution of 200 g. (1.44 moles) of potassium carbonate in 250 ml. of water at room temperature of about 25° C. over a period of 15 min. A precipitate formed after about 15 minutes. Stirring was continued until a thick paste formed and the mixture was then allowed to stand for another hour. The solid product was isolated by filtration, washed with small portions of water (amounting to a total of 500 ml.) and dried at 40° C. in a vacuum oven. Yield of 365 g. of a white crystalline powder (82% yield), m.p. 103° C. The material was of sufficient purity to be directly employed in polymerization and was employed in the polymerization described in Example 2 hereinafter. If desired, further purification can be attained through recrystallization from benzene or toluene.

후처리

  1. customA precipitate formed after about 15 minutes
  2. customformed
  3. waitto stand for another hour
  4. customThe solid product was isolated by filtration
  5. washwashed with small portions of water (amounting to a total of 500 ml
  6. custom) and dried at 40° C. in a vacuum oven

출처 및 근거

ORD 기록
ord-648c20a8b2b74d7796dc575fd812d837
출처 데이터셋
uspto-grants-1982_09
특허 번호
US04350801

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