Hydrochloric Acid → (1S,3aS,5S,7aR)-1-[(E)-2-aminoethoxyiminomethyl]-7a-methyl-5-phenyl-2,3,4,5,6,7-hexahydro-1H-inden-3a-ol

HRID 725175ノート

反応式

HRID 725175 の反応式
Cl.Cl.[NH2:3][CH2:4][CH2:5][O:6][NH2:7].C([O-])(=O)C.[Na+].Cl.[CH:14]([C@@H:16]1[C@:24]2([CH3:25])[C@@:19]([OH:32])([CH2:20][C@@H:21]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH2:22][CH2:23]2)[CH2:18][CH2:17]1)=O.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.O>[NH2:3][CH2:4][CH2:5][O:6]/[N:7]=[CH:14]/[C@@H:16]1[C@:24]2([CH3:25])[C@@:19]([OH:32])([CH2:20][C@@H:21]([C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=3)[CH2:22][CH2:23]2)[CH2:18][CH2:17]1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 517045Sodium AcetateHCID 11054353(1S,3aS,5S,7aR)-1-formyl-5-phenyl-7a-methylperhydroinden-3a-olHCID 143623262-(O-aminooxy)ethylamine dihydrochloride

生成物 1

HCID 10958069(1S,3aS,5S,7aR)-1-[(E)-2-aminoethoxyiminomethyl]-7a-methyl-5-phenyl-2,3,4,5,6,7-hexahydro-1H-inden-3a-ol収率 69.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 6.30 g of 0.12 g of 2-aminoethoxyamine dihydrochloride, 0.28 g of sodium acetate in 2 ml of dioxane and 1 ml of water was made aid to pH 4.5 with 3N HCl. A solution of 0.20 g of (1S,3aS,5S,7aR)-1-formyl-5-phenyl -7a-methylperhydroinden-3a-ol in 1 ml of dioxane and 0.5 ml of water was added dropwise at room temperature. After 1 hr the solution was alkalinized with 10% aqueous Na2CO3 and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and evaporated to dryness. The crude product was ground with diethyl ether to give 0.17 g of the title compound (I-am) as a white solid.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customevaporated to dryness

出典と根拠

ORDレコード
ord-0ed5ac84fe694c92b3957fa6fcc6899b
出典データセット
uspto-grants-1998_01
特許番号
US05705531

反応ノート

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