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

HRID 1684035노트

반응식

HRID 1684035 반응식
[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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-4ae30ea1d7234c1ca0c32e4ea68bea59
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05639782

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