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Acrylamide → HCID 13797271、化合物

HRID 1906070
ノート
印刷プレビュー

反応式

HRID 1906070 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 13797271HCID 13797271、化合物収率 79.2%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回
HCID 6228
Dimethylformamide
溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-dd09fb38961c49f6ae1aededd412cdb2
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04649219

反応ノート

読み込み中…

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