Pyridine → (S)-3-[(S)-2-(4-Acetoxy-phenyl)-2,3-dihydro-benzo[1,4]dioxin-6-yl]-2-((S)-1-phenyl-propylamino)-propionic acid methyl ester

HRID 391798ノート

反応式

HRID 391798 の反応式
[CH3:1][O:2][C:3](=[O:33])[C@@H:4]([NH:23][C@H:24]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:25][CH3:26])[CH2:5][C:6]1[CH:22]=[CH:21][C:9]2[O:10][C@@H:11]([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=3)[CH2:12][O:13][C:8]=2[CH:7]=1.N1C=CC=CC=1.[C:40](OC(=O)C)(=[O:42])[CH3:41]>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:33])[C@@H:4]([NH:23][C@H:24]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[CH2:25][CH3:26])[CH2:5][C:6]1[CH:22]=[CH:21][C:9]2[O:10][C@@H:11]([C:14]3[CH:15]=[CH:16][C:17]([O:20][C:40](=[O:42])[CH3:41])=[CH:18][CH:19]=3)[CH2:12][O:13][C:8]=2[CH:7]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 58327220(S)-3-[(S)-2-(4-Hydroxy-phenyl)-2,3-dihydro-benzo[1,4]dioxin-6-yl]-2-((S)-1-phenyl-propylamino)-propionic acid methyl ester

生成物 1

HCID 58327474(S)-3-[(S)-2-(4-Acetoxy-phenyl)-2,3-dihydro-benzo[1,4]dioxin-6-yl]-2-((S)-1-phenyl-propylamino)-propionic acid methyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of (S)-3-[(S)-2-(4-hydroxy-phenyl)-2,3-dihydro-benzo[1,4]dioxin-6-yl]-2-((S)-1-phenyl-propylamino)-propionic acid methyl ester (120 mg) in DCM (3 mL) was added pyridine at 0° C. To this mixture was added acetic anhydride. The mixture was stirred for 2-3 h. After completion of the reaction, the mixture was diluted with DCM (20 mL) and was washed with water, 1N HCl and brine solution. The organic layer was dried and concentrated to get the desired product as a white solid (110 mg). LCMS (m/z): 491.

後処理

  1. customAfter completion of the reaction
  2. washwas washed with water, 1N HCl and brine solution
  3. customThe organic layer was dried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-38281b3da87d487c94976c57cac73b0f
出典データセット
uspto-grants-2013_02
特許番号
US08383644B2

反応ノート

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