Dichloromethane → HCID 14324551, compound

HRID 1087668Notes

Reaction equation

HRID 1087668 reaction equation
[N+:1]([C:4]1[CH:5]=[C:6]([S:11](Cl)(=[O:13])=[O:12])[CH:7]=[CH:8][C:9]=1[Cl:10])([O-:3])=[O:2].ClCCl.[CH2:18]([NH2:34])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]>C(N(CC)CC)C>[CH2:18]([NH:34][S:11]([C:6]1[CH:7]=[CH:8][C:9]([Cl:10])=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)(=[O:13])=[O:12])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]

Participants

5

Reactant 3

HCID 6344Dichloromethane2×HCID 7323Benzenesulfonyl chloride, 4-chloro-3-nitro-HCID 8926Hexadecylamine

Product 1

HCID 14324551HCID 14324551, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

800 g of 3-nitro 4-chlorobenzenesulfonylchloride and 1,000 ml of dichloromethane were mixed. A dichloromethane solution of 600 g of hexadecylamine and 251 ml of triethylamine was added dropwise to the mixture. After the reaction was finished, the reaction solvent was removed under reduced pressure. 3,000 ml of methanol was added to the system. The mixture was then heated so that dissolution was effected. The solution was then gradually cooled. As a result, crystals precipitated. The crystals were then filtered off, and dried.

Workup

  1. customthe reaction solvent was removed under reduced pressure
  2. addition3,000 ml of methanol was added to the system
  3. temperatureThe mixture was then heated so that dissolution
  4. temperatureThe solution was then gradually cooled
  5. customAs a result, crystals precipitated
  6. filtrationThe crystals were then filtered off
  7. customdried

Sources & evidence

ORD record
ord-f3af51b3dba54180ae028070c669f4e7
Source dataset
uspto-grants-1990_10
Patent number
USH0000830

Reaction notes

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