Cyclohexylamine → HCID 178527177, compound

HRID 2210454Notes

Reaction equation

HRID 2210454 reaction equation
CS[C:3]1[NH:8][C:7]2[CH:9]=[CH:10][N:11]=[CH:12][C:6]=2[S:5](=[O:14])(=[O:13])[N:4]=1.[CH:15]1([NH2:21])[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1>>[CH:15]1([NH:21][C:3]2[NH:8][C:7]3[CH:9]=[CH:10][N:11]=[CH:12][C:6]=3[S:5](=[O:14])(=[O:13])[N:4]=2)[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1

Participants

3

Reactant 2

HCID 7965CyclohexylamineHCID 15651240HCID 15651240, compound

Product 1

HCID 178527177HCID 178527177, compound

Procedure

A solution of 0.7 g of 3-methylthio-4H- pyrido[4,3-e][1,2,4]thiadiazine 1,1-dioxide in 7 cm3 of cyclohexylamine is heated at reflux for 4 hours. The reaction mixture is concentrated under partial vacuum and the residue is taken up in 10 cm3 of water and is slightly basified by addition of 10% sodium hydroxide solution. The aqueous phase is stirred with 25 cm3 of diethyl ether in order to extract a possible excess of cyclohexylamine. After separation by settling, the aqueous solution is adjusted to a pH of 7 and the white precipitate is collected on a filter and washed with water. It is recrystallized from hot water.

Workup

  1. temperatureat reflux for 4 hours
  2. concentrationThe reaction mixture is concentrated under partial vacuum
  3. additionis slightly basified by addition of 10% sodium hydroxide solution
  4. extractionto extract a possible excess of cyclohexylamine
  5. customAfter separation
  6. customthe white precipitate is collected on
  7. filtrationa filter
  8. washwashed with water
  9. customIt is recrystallized from hot water

Sources & evidence

ORD record
ord-6c59e526ebcf484e8d8ed668db9a4985
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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