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Water → methyl 2-(4-chloro-3-((2-chloro-4-(((2S)-4-methyl-3,4-dihydro-2H-1,4-benzoxazin-2-yl)methoxy)benzoyl)amino)phenyl)-2-methylpropanoate

HRID 1818689
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HRID 1818689 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([O:11][CH2:12][C@@H:13]2[CH2:18][N:17]([CH3:19])[C:16]3[CH:20]=[CH:21][CH:22]=[CH:23][C:15]=3[O:14]2)[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[NH2:24][C:25]1[CH:26]=[C:27]([C:32]([CH3:38])([CH3:37])[C:33]([O:35][CH3:36])=[O:34])[CH:28]=[CH:29][C:30]=1[Cl:31].N1C=CC=CC=1.O>ClCCl>[Cl:31][C:30]1[CH:29]=[CH:28][C:27]([C:32]([CH3:37])([CH3:38])[C:33]([O:35][CH3:36])=[O:34])=[CH:26][C:25]=1[NH:24][C:4](=[O:5])[C:3]1[CH:7]=[CH:8][C:9]([O:11][CH2:12][C@@H:13]2[CH2:18][N:17]([CH3:19])[C:16]3[CH:20]=[CH:21][CH:22]=[CH:23][C:15]=3[O:14]2)=[CH:10][C:2]=1[Cl:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 23125543HCID 23125543, 화합물HCID 86609826HCID 86609826, 화합물

생성물 1

HCID 66782455methyl 2-(4-chloro-3-((2-chloro-4-(((2S)-4-methyl-3,4-dihydro-2H-1,4-benzoxazin-2-yl)methoxy)benzoyl)amino)phenyl)-2-methylpropanoate

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

A solution of the compound prepared in Example 17 in dichloromethane (1.8 mL) was dropped to a solution of the compound (100 mg) prepared in Example 16 in dichloromethane (1.8 mL). Pyridine (0.057 mL) was added to the reaction mixture, which was stirred for 1 hour at room temperature. The reaction mixture dissolved to water was extracted with ethyl acetate. The organic layer was sequentially washed with diluted hydrochloric acid, saturated sodium hydrogencarbonate solution, and saturated brine solution and was dried by anhydrous magnesium sulphate. The title compound (164 mg) having the following physical data was obtained by purifying the residue obtained by removing the solvent by silica gel column chromatography (n-hexane:ethyl acetate=4:1). TLC: Rf 0.41 (n-hexane:ethyl acetate=2:1).

후처리

  1. extractionwas extracted with ethyl acetate
  2. washThe organic layer was sequentially washed with diluted hydrochloric acid, saturated sodium hydrogencarbonate solution, and saturated brine solution
  3. dry with materialwas dried by anhydrous magnesium sulphate
  4. customwas obtained
  5. customby purifying the residue
  6. customobtained
  7. customby removing the solvent by silica gel column chromatography (n-hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-7c0d61b17cb24852a8481931318f38b2
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07601712B2

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