海萝胶 → hexamethylene bis(thiosulphate)N-tert-butyl-N-benzylammonium salt

HRID 463540

反应方程式

HRID 463540 反应方程式
Cl[CH2:2][CH:3]1CC[CH:6]([CH2:9]Cl)[CH2:5][CH2:4]1.O.O.O.O.O.[S:16]([O-:20])([O-:19])(=[O:18])=[S:17].[Na+].[Na+].[C:23]([NH:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([CH3:26])([CH3:25])[CH3:24].Cl.[S:36]([O-:40])([O-:39])(=[O:38])=[S:37]>CO.O>[C:23]([NH2+:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([CH3:26])([CH3:24])[CH3:25].[S:16]([O-:20])([O:19][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:9][O:39][S:36]([O-:40])(=[O:38])=[S:37])(=[O:18])=[S:17].[C:23]([NH2+:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([CH3:26])([CH3:24])[CH3:25]

参与物

8

反应物 5

HCID 313海萝胶HCID 1084Thiosulfate ionHCID 61475五水硫代硫酸钠HCID 69992Cyclohexane, 1,4-bis(chloromethyl)-HCID 76908N-叔丁基苄胺

产物 1

HCID 131714228hexamethylene bis(thiosulphate)N-tert-butyl-N-benzylammonium salt

试剂、催化剂与溶剂 2

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂2 次HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂3 次

反应条件

温度
135 °C

实验过程

1,4-bis(chloromethyl)cyclohexane (0.165 mole), sodium thiosulphate pentahydrate (0.369 mole) sodium sulfite (6.1 g), methanol (150 ml) and water (150 ml) were charged into an autoclave and heated at 135° C. for 45 minutes. To the cooled reaction mixture, which was a solution of 1,4-dimethylcyclohexane-α,α-bis(thiosulphate)sodium salt, 400 ml of water was added. N-tert-butylbenzylamine (0.306 mole) in 150 ml methanol and 850 ml H2O was adjusted with concentrated HCl to pH4, and the resulting solution was added with stirring to the thiosulphate solution. The white precipitate was filtered, washed with water and dried. Yield: 92 g, (91%) of 1,4-dimethylcyclohexane-α,α-bis(thiosulphate)N-tert-butyl, N-benzylammonium salt.

后处理

  1. customTo the cooled reaction mixture, which
  2. additionwas added
  3. additionthe resulting solution was added
  4. filtrationThe white precipitate was filtered
  5. washwashed with water
  6. customdried

来源与证据

ORD记录
ord-32b8be04b6174a2580d656012a7d1254
来源数据集
uspto-grants-1985_05
专利号
US04520154

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