N-methyl-2-pyrrolidone → HCID 135593826, compound

HRID 1680494Notes

Reaction equation

HRID 1680494 reaction equation
[Na].[OH:2][C:3]1[CH:12]=[CH:11][C:10]([N:13]=[N:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:16]=2[S:24]([CH3:27])(=[O:26])=[O:25])=[C:9]2[C:4]=1[CH:5]=[CH:6][CH:7]=[C:8]2[NH:28][S:29]([C:32]1[CH:33]=[C:34]([S:38]([OH:41])(=[O:40])=[O:39])[CH:35]=[CH:36][CH:37]=1)(=[O:31])=[O:30].CN1CCCC1=O.P(Cl)(Cl)([Cl:51])=O>>[S:38]([Cl:51])([OH:41])(=[O:40])=[O:39].[OH:2][C:3]1[CH:12]=[CH:11][C:10]([N:13]=[N:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:16]=2[S:24]([CH3:27])(=[O:26])=[O:25])=[C:9]2[C:4]=1[CH:5]=[CH:6][CH:7]=[C:8]2[NH:28][S:29]([C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1)(=[O:30])=[O:31]

Participants

5

Reactant 4

HCID 13387N-methyl-2-pyrrolidoneHCID 24813Phosphorus oxychlorideHCID 5360545SodiumHCID 135593825HCID 135593825, compound

Product 1

HCID 135593826HCID 135593826, compound

Conditions

Temperature
60 °C

Procedure

126 g of the sodium salt of 3-[5-hydroxy-8-(2-methylsulphonyl-4-nitrophenylazo)-naphthylsulphamoyl]-benzene sulphonic acid are stirred in 700 ml of phosphorus oxychloride and heated to 60° C. At this temperature 20 g of N-methylpyrrolidone are gradually added, whereupon the mixture is stirred at 60° C. for 6 h and thereafter allowed to cool. The precipitate formed is filtered with suction, washed with dichloroethane and dried.

Workup

  1. temperatureto cool
  2. customThe precipitate formed
  3. filtrationis filtered with suction
  4. washwashed with dichloroethane
  5. customdried

Sources & evidence

ORD record
ord-8c128486c32a442eb451b88f8b056c43
Source dataset
uspto-grants-1981_06
Patent number
US04273855

Reaction notes

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