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4-Methylmorpholine → HCID 11582801、化合物

HRID 908958
ノート
印刷プレビュー

反応式

HRID 908958 の反応式
[C:1]1([CH2:7][CH2:8][CH2:9][NH2:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN1CCOCC1.C1(N=C=NC2CCCCC2)CCCCC1.[CH3:33][N:34]([CH3:52])[C:35]1([C:45]2[CH:50]=[CH:49][CH:48]=[C:47]([F:51])[CH:46]=2)[CH2:40][CH2:39][C:38](=[CH:41][C:42](O)=[O:43])[CH2:37][CH2:36]1.[OH-].[Na+]>CN(C)C=O.O>[CH3:52][N:34]([CH3:33])[C:35]1([C:45]2[CH:50]=[CH:49][CH:48]=[C:47]([F:51])[CH:46]=2)[CH2:40][CH2:39][C:38](=[CH:41][C:42]([NH:10][CH2:9][CH2:8][CH2:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[O:43])[CH2:37][CH2:36]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 79724-MethylmorpholineHCID 10868DicyclohexylcarbodiimideHCID 14798Sodium HydroxideHCID 162593-PhenylpropylamineHCID 67386283[4-Dimethylamino-4-(3-fluoro-phenyl)-cyclohexylidene]acetic acid

生成物 1

HCID 11582801HCID 11582801、化合物収率 29%

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

3-phenylpropylamine (768 mg, 5.68 mmol), N-methylmorpholine (1.15 g, 11.36 mmol) and dicyclohexylcarbodiimide (2.34 g, 11.36 mmol) were added to a solution of [4-dimethylamino-4-(3-fluoro-phenyl)-cyclohexylidene]acetic acid (1.5 g, 5.68 mmol) in dry dimethylformamide (35 ml) under argon and the mixture was stirred at RT for 3 d. The urea which had precipitated out was separated off and the filtrate was introduced into a mixture of saturated NaCl solution (40 ml) and saturated NaHCO3 solution (10 ml). Still further urea thereby precipitated out and was separated off. The aqueous phase was diluted with water (300 ml), 5 M sodium hydroxide solution (7 ml, 35 mmol) was added and the mixture was stored at 5° C. for 20 h. The crude product thereby precipitated out as a beige-coloured solid (2.16 g). After chromatography on silica gel G [100 g; EtOAc/MeOH (10:1)], the amide was obtained in a yield of 29% (648.5 mg) with an m.p. of 129-131° C.

後処理

  1. customThe urea which had precipitated out
  2. customwas separated off
  3. additionthe filtrate was introduced into a mixture of saturated NaCl solution (40 ml) and saturated NaHCO3 solution (10 ml)
  4. customStill further urea thereby precipitated out and
  5. customwas separated off
  6. additionwas added
  7. waitthe mixture was stored at 5° C. for 20 h
  8. customThe crude product thereby precipitated out as a beige-coloured solid (2.16 g)

出典と根拠

ORDレコード
ord-96fe3e817ef7482d85716aea86e885fa
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08017630B2

反応ノート

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