Triethylamine → HCID 21476308, 화합물

HRID 2293105노트

반응식

HRID 2293105 반응식
C(N(CC)CC)C.[NH2:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH2:20][CH2:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1.[CH2:26]([S:29](Cl)(=[O:31])=[O:30])[CH2:27][CH3:28]>CN1CCN(C)C1=O.O1CCCC1>[CH2:26]([S:29]([NH:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH2:20][CH2:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1)(=[O:31])=[O:30])[CH2:27][CH3:28]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 662791-Propanesulfonyl chlorideHCID 21476304HCID 21476304, 화합물

생성물 1

HCID 21476308HCID 21476308, 화합물수율 61.7%

시약·촉매·용매 2

HCID 66611,3-Dimethyl-2-imidazolidinone용매HCID 8028Tetrahydrofuran용매

실험 절차

5.53 g of triethylamine was added to 6.03 g of 2-aminomethyl-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane suspended in 60 ml of 1,3-dimethyl-2-imidazolidinone, and then 5.10 g of propanesulfonyl chloride dissolved in 20 ml of tetrahydrofuran was added to the mixture. The resulting mixture was stirred at room temperature for 30 minutes. The reaction mixture was poured into ice water, and crystals precipitated were collected by filtration. The precipitated crystals were recrystallized from methanol-acetonitrile to obtain 5.34 g of 2-(propylsulfonylaminomethyl)-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane

후처리

  1. additionwas added to the mixture
  2. customprecipitated
  3. filtrationwere collected by filtration
  4. customThe precipitated crystals were recrystallized from methanol-acetonitrile

출처 및 근거

ORD 기록
ord-d04d03f739b44764a609e864c48331e4
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05686452

반응 노트

불러오는 중…