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Sodium Hydroxide → HCID 21105604, 화합물

HRID 2426646
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HRID 2426646 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH3:23])[C:9](=[O:22])[C:10]2[CH:15]=[CH:14][C:13]([CH:16]3[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]3)=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.P([O-])([O-])([O-])=O.[Na+].[Na+].[Na+].[Br:32][CH:33]([CH2:37][CH2:38]Cl)[C:34](Br)=[O:35].[OH-].[Na+]>C(#N)C.O>[Br:32][CH:33]1[CH2:37][CH2:38][N:1]([C:2]2[CH:7]=[CH:6][C:5]([N:8]([CH3:23])[C:9](=[O:22])[C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]4)=[CH:12][CH:11]=3)=[CH:4][CH:3]=2)[C:34]1=[O:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium Hydroxide2회HCID 24243Trisodium PhosphateHCID 110327462-Bromo-4-chlorobutyryl bromideHCID 21105617HCID 21105617, 화합물

생성물 1

HCID 21105604HCID 21105604, 화합물

시약·촉매·용매 2

HCID 962Water용매2회
HCID 6342Acetonitrile용매

실험 절차

N-(4-Aminophenyl)-4-cyclohexyl-N-methylbenzamide (3.0 g) in acetonitrile (30 ml) was mixed with trisodium phosphate (0.95 g) and, at 0° C., 2-bromo-4-chlorobutyryl bromide (2.9 g) was added. After one hour, a solution of sodium hydroxide (0.85 g) in water (10 ml) was added and the mixture was stirred vigorously at room temperature for 6 hours. The same amount of sodium hydroxide solution was then added, and stirring was continued for 48 hours. The reaction solution was diluted with water and extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and concentrated. The residue was purified by chromatography on silica gel (mobile phase ethyl acetate/heptane 1:2). This resulted in the product with the molecular weight of 455.40 (C24H27BrN2O2); MS (ESI): 456 (M+H+).

후처리

  1. stirringstirring
  2. waitwas continued for 48 hours
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography on silica gel (mobile phase ethyl acetate/heptane 1:2)
  7. customThis resulted in the product with the molecular weight of 455.40 (C24H27BrN2O2)

출처 및 근거

ORD 기록
ord-e86ca7d9e38543bbbfb490f8da321a12
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07968550B2

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