Calcium Chloride → trans-2-(5-Amino-3,4-dimethoxyphenyl)-4-(3,4,5-trimethoxy-phenyl)-1,3-dithiolane

HRID 1684035ノート

反応式

HRID 1684035 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C@H:14]2[S:18][C@H:17]([C:19]3[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH3:28])=[C:21]([O:29][CH3:30])[CH:20]=3)[CH2:16][S:15]2)[CH:6]=[C:7]([N+:11]([O-])=O)[C:8]=1[O:9][CH3:10].[Cl-].[Ca+2].[Cl-]>C(O)C.O.[Zn]>[NH2:11][C:7]1[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=[C:5]([C@H:14]2[S:18][C@H:17]([C:19]3[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH3:28])=[C:21]([O:29][CH3:30])[CH:20]=3)[CH2:16][S:15]2)[CH:6]=1

参加物

6

反応物 2

HCID 5284359Calcium ChlorideHCID 86750974trans-2-(3,4-Dimethoxy-5-nitrophenyl)-4-(3,4,5-trimethoxyphenyl)-1,3-dithiolane

生成物 1

HCID 86750975trans-2-(5-Amino-3,4-dimethoxyphenyl)-4-(3,4,5-trimethoxy-phenyl)-1,3-dithiolane

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Trans-2-(3,4-dimethoxy-5-nitrophenyl)-4-(3,4,5-trimethoxyphenyl)-1,3-dithiolane (2) (FIG. 20) (3.10 g, 6.84 mmole) was predissolved in 33 ml absolute ethanol. To this solution was added calcium chloride (0.721 g, 6.50 mmole) predissolved in 7 ml H2O followed by freshly activated zinc dust (10.0 g,195 mmole). The reaction was refluxed for 12 hours. The solid was removed by vacuum filtration through celite and was washed with ethyl acetate. The filtrate was washed with H2O, dried over MgSO4, and evaporated in vacuo to a white foam (2.52 g, 87%).

後処理

  1. temperatureThe reaction was refluxed for 12 hours
  2. customThe solid was removed by vacuum filtration through celite
  3. washwas washed with ethyl acetate
  4. washThe filtrate was washed with H2O
  5. dry with materialdried over MgSO4
  6. customevaporated in vacuo to a white foam (2.52 g, 87%)

出典と根拠

ORDレコード
ord-4ae30ea1d7234c1ca0c32e4ea68bea59
出典データセット
uspto-grants-1997_06
特許番号
US05639782

反応ノート

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