Calcium Chloride → Trans-2-(4-allyloxy-5-amino-3-methoxyphenyl)-4-(3,4,5-trimeth-oxyphenyl)-1,3-dithiolane

HRID 260977ノート

反応式

HRID 260977 の反応式
[CH2:1]([O:4][C:5]1[C:10]([N+:11]([O-])=O)=[CH:9][C:8]([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:7][C:6]=1[O:31][CH3:32])[CH:2]=[CH2:3].[Cl-].[Ca+2].[Cl-]>C(O)C.O.[Zn]>[CH2:1]([O:4][C:5]1[C:10]([NH2:11])=[CH:9][C:8]([C@H:14]2[S:18][C@H:17]([C:19]3[CH:20]=[C:21]([O:29][CH3:30])[C:22]([O:27][CH3:28])=[C:23]([O:25][CH3:26])[CH:24]=3)[CH2:16][S:15]2)=[CH:7][C:6]=1[O:31][CH3:32])[CH:2]=[CH2:3]

参加物

6

反応物 2

HCID 5284359Calcium ChlorideHCID 86749584Trans-2-(4-allyloxy-3-methoxy-5-nitrophenyl)-4-(3,4,5-trimethoxyphenyl)-1,3-dithiolane

生成物 1

HCID 86749585Trans-2-(4-allyloxy-5-amino-3-methoxyphenyl)-4-(3,4,5-trimeth-oxyphenyl)-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-(4-allyloxy-3-methoxy-5-nitrophenyl)-4-(3,4,5-trimethoxy-phenyl)-1,3-dithiolane (24) 2.60 g, 5.43 mmole) was predissolved in 33 ml absolute ethanol. To this solution was added calcium chloride (0.602 g, 5.43 mmole) predissolved in 7 ml H2O followed by freshly activated zinc dust (7.09 g, 108 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 10% NaHCO3, dried over MgSO4, and

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 10% NaHCO3
  5. dry with materialdried over MgSO4

出典と根拠

ORDレコード
ord-748b7a01d7264ac9a314cd52615b7bd7
出典データセット
uspto-grants-1996_06
特許番号
US05530141

反応ノート

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