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Acrylamide → HCID 13797271, 화합물

HRID 1906070
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HRID 1906070 반응식
[C:1]([NH2:5])(=[O:4])[CH:2]=[CH2:3].Br[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[OH-].[K+].C1C2NC3C(=CC=CC=3)SC=2C=CC=1>C1C=CC=CC=1.CN(C)C=O>[O:15]([CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH:5][C:1](=[O:4])[CH:2]=[CH2:3])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6579AcrylamideHCID 7108PhenothiazineHCID 14797Potassium HydroxideHCID 129593778-Phenoxyoctyl bromide

생성물 1

HCID 13797271HCID 13797271, 화합물수율 79.2%

시약·촉매·용매 2

HCID 241Benzene용매2회
HCID 6228
Dimethylformamide
용매

실험 절차

Added to 20 ml of N,N-dimethylformamide were 0.62 g of acrylic amide and 2.0 g of (8-bromooctyloxy)benzene. With stirring, 0.49 g of flaky potassium hydroxide which had been ground in a mortar was added. Phenothiazine was added in an amount of 0.5% based on the acrylic amde. After they were reacted at 0°-5° C. for 6 hours, insoluble filtered off from the liquid reaction mixture. The solvent and unreacted raw materials were distilled off from the filtrate. The residue was extracted with benzene-water, thereby obtaining the intended product in the benzene layer. Benzene was then driven off from the benzene layer to obtain 1.53 g of N-(8-phenoxyoctyl)acrylic amide (yield: 79%). It was purified further with column chromatography in which silica gel and benzene were used as an adsorbent and developer respectively. Its melting point was measured and its elementary analysis was also conducted. The following results were obtained. Melting point: 45°-47° C. Elementary analysis data: C, 74.21% (Calculated: 74.14%); H, 9.09% (9.15 %); N, 5.12% (5.09%).

후처리

  1. additionwas added
  2. customAfter they were reacted at 0°-5° C. for 6 hours
  3. custominsoluble filtered off from the liquid reaction mixture
  4. distillationThe solvent and unreacted raw materials were distilled off from the filtrate
  5. extractionThe residue was extracted with benzene-water
  6. customobtaining the intended product in the benzene layer

출처 및 근거

ORD 기록
ord-dd09fb38961c49f6ae1aededd412cdb2
출처 데이터셋
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04649219

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