Triethylamine → 4,5-dichloro-6-[3-(phenylthio)propyloxy]-3(2H)-pyridazinone

HRID 1451229노트

반응식

HRID 1451229 반응식
Br[CH2:2][CH2:3][CH2:4][S:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl:12][C:13]1[C:14](=[O:21])[NH:15][N:16]=[C:17]([OH:20])[C:18]=1[Cl:19].C(N(CC)CC)C>CN(C)C=O>[Cl:12][C:13]1[C:14](=[O:21])[NH:15][N:16]=[C:17]([O:20][CH2:2][CH2:3][CH2:4][S:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:18]=1[Cl:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 70618473-Bromopropyl phenyl sulfideHCID 178518839HCID 178518839, 화합물

생성물 1

HCID 199743804,5-dichloro-6-[3-(phenylthio)propyloxy]-3(2H)-pyridazinone수율 66.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

After 1.57 g of 1-bromo-3-phenylthiopropane, 2 g of 4,5-dichloro-6-hydroxy-3(2H)-pyridazinone and 1.3 g of triethylamine were dissolved in dimethylformamide, the mixture was stirred at room temperature for 24 hours. The reaction mixture was poured onto water. The formed crystals were taken by filtration and thoroughly washed with water. The crystals were recrystallized from ethanol to give 1.5 g of the objective compound. Yield, 52%, Melting point, 187°-188° C.

후처리

  1. additionThe reaction mixture was poured onto water
  2. filtrationThe formed crystals were taken by filtration
  3. washthoroughly washed with water
  4. customThe crystals were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-ce26d6e61583406e996a61aab7cd2a1a
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05604226

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