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

HRID 260977노트

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HRID 260977 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

HCID 86749585Trans-2-(4-allyloxy-5-amino-3-methoxyphenyl)-4-(3,4,5-trimeth-oxyphenyl)-1,3-dithiolane

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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

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 10% NaHCO3
  5. dry with materialdried over MgSO4

출처 및 근거

ORD 기록
ord-748b7a01d7264ac9a314cd52615b7bd7
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530141

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