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

HRID 1451229ノート

反応式

HRID 1451229 の反応式
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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 70618473-Bromopropyl phenyl sulfideHCID 178518839HCID 178518839、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ce26d6e61583406e996a61aab7cd2a1a
出典データセット
uspto-grants-1997_02
特許番号
US05604226

反応ノート

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