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Dichloromethane → HCID 14653252, 화합물

HRID 893306
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HRID 893306 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 531671-MethylpiperazineHCID 14653249HCID 14653249, 화합물

생성물 1

HCID 14653252HCID 14653252, 화합물수율 101%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa29c80a62ac44a98a77d5b104d1e05e
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05124331

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