Dichloromethane → HCID 73794037, compound

HRID 1414847Notes

Reaction equation

HRID 1414847 reaction equation
[CH3:1][S:2][CH2:3][S:4]([CH3:6])=[O:5].[H-].[K+].[C:9](#[N:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(Cl)Cl>COCCOC.O>[CH3:6][S:4]([C:3]([S:2][CH3:1])=[C:9]([NH2:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:5]

Participants

7

Procedure

1.753 Grams of methyl methylthiomethyl sulfoxide was dissolved in 20 ml of 1,2-dimethoxyethane, and to the solution 580 mg of potassium hydride was added under cooling with ice, and the system was stirred for one and half hours at room temperature. Upon addition of 1.460g of benzonitrile and subsequent stirring for 15 hours at room temperature and for one hour at 50° C., the system was added with 70 ml of methylene chloride and 2 ml of water, followed by stirring for one hour at room temperature. The mixture was dried with Glauber's salt, and filtrated. The filtrate was concentrated under reduced pressure and the resulting yellow solid was crystallized from methylene chloride-carbon tetrachloride-cyclohexane to obtain 2.208g of 1-methylsulfinyl-1-methylthio-2-amino-2-phenylethylene. The isolation yield was 69%.

Workup

  1. temperatureunder cooling with ice
  2. stirringsubsequent stirring for 15 hours at room temperature and for one hour at 50° C.
  3. stirringby stirring for one hour at room temperature
  4. dry with materialThe mixture was dried with Glauber's salt
  5. filtrationfiltrated
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customthe resulting yellow solid was crystallized from methylene chloride-carbon tetrachloride-cyclohexane

Sources & evidence

ORD record
ord-7dad9771b8434bf1a9f0068ece0f6f15
Source dataset
uspto-grants-1977_01
Patent number
US04002682

Reaction notes

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