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

HRID 463540

반응식

HRID 463540 반응식
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]

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매3회

반응 조건

온도
135 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-32b8be04b6174a2580d656012a7d1254
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04520154

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