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4-Methylmorpholine → HCID 11582801, 화합물

HRID 908958
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HRID 908958 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

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

생성물 1

HCID 11582801HCID 11582801, 화합물수율 29%

시약·촉매·용매

2
HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-96fe3e817ef7482d85716aea86e885fa
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08017630B2

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