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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
ノート
印刷プレビュー

反応式

HRID 1818689 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 23125543HCID 23125543、化合物HCID 86609826HCID 86609826、化合物

生成物 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

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-7c0d61b17cb24852a8481931318f38b2
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07601712B2

反応ノート

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