Hydrochloric Acid → hexamethylene bis(thiosulphate)N-tert-butyl-N-benzylammonium salt

HRID 463540

反応式

HRID 463540 の反応式
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]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 1084Thiosulfate ionHCID 61475Sodium Thiosulfate PentahydrateHCID 69992Cyclohexane, 1,4-bis(chloromethyl)-HCID 76908N-(1,1-Dimethylethyl)benzenemethanamine

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒3 回

反応条件

温度
135 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32b8be04b6174a2580d656012a7d1254
出典データセット
uspto-grants-1985_05
特許番号
US04520154

関連ノート

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