Chlorosulfonic acid → HCID 14653249, compound

HRID 893304Notes

Reaction equation

HRID 893304 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[N:10]=[C:9]1[CH3:18].[Cl:19][S:20](O)(=[O:22])=[O:21]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[C:16]([S:20]([Cl:19])(=[O:22])=[O:21])[S:17][C:11]=2[N:10]=[C:9]1[CH3:18]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 901565HCID 901565, compound

Product 1

HCID 14653249HCID 14653249, compound

Procedure

To 140 ml of chlorosulfonic acid was added little by little 54.8 g of 3,4-dihydro-3-(2-chlorophenyl)-2-methyl-4-oxothieno[2,3-d]pyrimidine. After the mixture was heated at 70°-75° C. on the oil bath and stirred for 1.5 hours, the reaction mixture was cooled and then poured onto 2 l of icewater carefully. The precipitated crystals were collected by suction-filtration to afford 65 g of the title compound, m.p. 172°-174° C.

Workup

  1. temperatureAfter the mixture was heated at 70°-75° C. on the oil bath
  2. temperaturethe reaction mixture was cooled
  3. additionpoured onto 2 l of icewater carefully
  4. filtrationThe precipitated crystals were collected by suction-filtration

Sources & evidence

ORD record
ord-31f4834126e947aeb95f8fbd52a75989
Source dataset
uspto-grants-1992_06
Patent number
US05124331

Reaction notes

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