Tetramethylammonium Hydroxide Pentahydrate → (+/-)-alpha-tert.Butyloxycarbonylamino-3-(4'-chloro-5-(diethoxyphosphinyl)methyl-[1.1'-biphenyl]-3-yl) propanoic acid cinnamyl ester

HRID 1109453

反応式

HRID 1109453 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:13][C:14]1[CH:15]=[C:16]([C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=2)[CH:17]=[C:18]([CH2:20][P:21]([O:26][CH2:27][CH3:28])([O:23][CH2:24][CH3:25])=[O:22])[CH:19]=1)[C:10]([OH:12])=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].O.O.O.O.O.[OH-].C[N+](C)(C)C.[CH2:47](Br)[CH:48]=[CH:49][C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1>CN(C)C=O>[CH2:47]([O:11][C:10](=[O:12])[CH:9]([NH:8][C:6]([O:5][C:1]([CH3:3])([CH3:4])[CH3:2])=[O:7])[CH2:13][C:14]1[CH:15]=[C:16]([C:29]2[CH:30]=[CH:31][C:32]([Cl:35])=[CH:33][CH:34]=2)[CH:17]=[C:18]([CH2:20][P:21]([O:26][CH2:27][CH3:28])([O:23][CH2:24][CH3:25])=[O:22])[CH:19]=1)[CH:48]=[CH:49][C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1

参加物

5

反応物 3

HCID 82620Tetramethylammonium Hydroxide PentahydrateHCID 98116BromomethylstyreneHCID 14127515HCID 14127515、化合物

生成物 1

HCID 56990101(+/-)-alpha-tert.Butyloxycarbonylamino-3-(4'-chloro-5-(diethoxyphosphinyl)methyl-[1.1'-biphenyl]-3-yl) propanoic acid cinnamyl ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1.05 g of the product of step b) in 5 ml dimethylformamide are added 362 mg tetramethyl ammonium hydroxide pentahydrate. The mixture is stirred at room temperature 11/2 hours and then treated with 394 mg cinnamyl bromide. The mixture is stirred at room temperature 17 hours. The mixture is diluted with ice/water (about 50 ml) and extracted with diethyl ether. The extracts are washed with 10 ml aqueous 1N KHCO3 solution, dried (Na2SO4) and evaporated to give the heading compound as an oil.

後処理

  1. stirringThe mixture is stirred at room temperature 17 hours
  2. extractionextracted with diethyl ether
  3. washThe extracts are washed with 10 ml aqueous 1N KHCO3 solution
  4. dry with materialdried (Na2SO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-03ee18f2704e47f690db436e7429b7f1
出典データセット
uspto-grants-1994_06
特許番号
US05321016

関連ノート

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