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Triethylamine → 1-Nicotinoyl-3-phenyl-1,4,5,6-tetrahydropyridazine

HRID 2307259
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반응식

HRID 2307259 반응식
[C:1]1([C:7]2[CH2:12][CH2:11][CH2:10][NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[C:14](Cl)(=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[N:17][CH:16]=1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[C:14]([N:9]1[CH2:10][CH2:11][CH2:12][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8]1)(=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[N:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 106785433-phenyl-1,4,5,6-tetrahydropyridazine

생성물 1

HCID 98565971-Nicotinoyl-3-phenyl-1,4,5,6-tetrahydropyridazine수율 46.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

3-Phenyl-1,4,5,6-tetrahydropyridazine (2.4 g) synthesized in Reference Example 1 was dissolved in chloroform (50 ml). Thereto were added nicotinic acid chloride hydrochloride (2.6 g) and triethylamine (3.2 g) with ice-cooling. Stirring was conducted for 30 minutes. The reaction mixture was washed with water, dried over anhydrous sodium sulfate and then concentrated. The residue was purified by silica gel column chromatography to obtain 1.8 g of a title compound.

후처리

  1. temperaturecooling
  2. washThe reaction mixture was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-256cf26e12014ca682e793502cf1d3df
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06831083B2

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