Dichloromethane → HCID 14653252, compound

HRID 893306Notes

Reaction equation

HRID 893306 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]=[C:16]([S:18](Cl)(=[O:20])=[O:19])[S:17][C:11]=2[N:10]=[C:9]1[CH3:22].ClCCl.[CH3:26][N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1>C(N(CC)CC)C>[ClH:1].[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:18]([N:30]3[CH2:31][CH2:32][N:27]([CH3:26])[CH2:28][CH2:29]3)(=[O:20])=[O:19])[S:17][C:11]=2[N:10]=[C:9]1[CH3:22]

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 531671-MethylpiperazineHCID 14653249HCID 14653249, compound

Product 1

HCID 14653252HCID 14653252, compoundYield 101%

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

To 5.0 g of 3,4-dihydro-3-(2-chlorophenyl)-6-chlorosulfonyl-2-methyl-4-oxothieno[2,3-d]pyrimidine were added 80 ml of dichloromethane, 4.5 ml of triethylamine and 1.4 g of N-methylpiperazine, and the mixture was stirred at room temperature for 20 minutes. After the reaction mixture was washed with water, isopropyl alcohol saturated with hydrochloric acid gas was added to the concentrated residue to convert it into hydrochloride, which was recrystallized from methanol to afford 3.2 g of the title compound, m.p. 295°-297° C.

Workup

  1. washAfter the reaction mixture was washed with water, isopropyl alcohol saturated with hydrochloric acid gas
  2. additionwas added to the concentrated residue
  3. customwas recrystallized from methanol

Sources & evidence

ORD record
ord-fa29c80a62ac44a98a77d5b104d1e05e
Source dataset
uspto-grants-1992_06
Patent number
US05124331

Reaction notes

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