Dichloromethane → HCID 13209440, 화합물

HRID 620134

반응식

HRID 620134 반응식
[CH2:1]1[CH2:6][CH2:5][CH:4]([SH:7])[CH2:3][CH2:2]1.[C:8]1([N:14]2[C:19](=[O:20])[C:18]([Cl:21])=[C:17](Cl)[CH:16]=[N:15]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(Cl)Cl.[OH-].[Na+]>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.O>[C:8]1([N:14]2[C:19](=[O:20])[C:18]([Cl:21])=[C:17]([S:7][CH:4]3[CH2:5][CH2:6][CH2:1][CH2:2][CH2:3]3)[CH:16]=[N:15]2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 15290CyclohexanethiolHCID 728134,5-Dichloro-2-phenyl-3(2H)-pyridazinone

생성물 1

HCID 13209440HCID 13209440, 화합물

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매

실험 절차

38.3 parts by weight of cyclohexylthiol were added dropwise to a mixture of 72.3 parts by weight of 1-phenyl-4,5-dichloropyridazin-6-one in 300 parts by volume of methylene chloride, 3 parts by weight of triethylbenzylammonium chloride, and 13.2 parts by weight of sodium hydroxide in 150 parts by volume of water at room temperature (20° C.), and the reaction mixture was kept at this temperature for 12 hours, while stirring vigorously. The organic phase was separated off, washed with twice 100 parts by volume of water, dried and then concentrated. The residue was recrystallized from ethylacetate. 61 parts by weight of 1-phenyl-4-(cyclohexylthio)-5-chloropyridazin-6-one of melting point 125°-127° C. were obtained (compound A1).

후처리

  1. customThe organic phase was separated off
  2. washwashed with twice 100 parts by volume of water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from ethylacetate

출처 및 근거

ORD 기록
ord-387bee3514944a32aca67878a6c70e42
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04820704

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