Sodium hydride → 3-(3-Amino-3-methylbutoxy)-6-chloropyridazine

HRID 745505

반응식

HRID 745505 반응식
[H-].[Na+].[Cl:3][C:4]1[N:5]=[N:6][C:7](Cl)=[CH:8][CH:9]=1.[NH2:11][C:12]([CH3:17])([CH3:16])[CH2:13][CH2:14][OH:15]>CCOCC.C1C=CC=CC=1.C(O)(C)(C)C>[NH2:11][C:12]([CH3:17])([CH3:16])[CH2:13][CH2:14][O:15][C:7]1[N:6]=[N:5][C:4]([Cl:3])=[CH:9][CH:8]=1

참가 물질

7

반응물 3

HCID 24758Sodium hydrideHCID 673313,6-DichloropyridazineHCID 6410003-Amino-3-methylbutan-1-ol

생성물 1

HCID 100362353-(3-Amino-3-methylbutoxy)-6-chloropyridazine수율 84.8%

시약·촉매·용매 3

HCID 241Benzene용매2회HCID 3283Diethyl Ether용매HCID 6386tert-Butanol용매

실험 절차

A mixture of 0.62 g of 60% sodium hydride, 1.91 g of 3,6-dichloropyridazine and 10 ml of benzene was stirred while being cooled with ice, and a solution consisting of 1.32 g of 3-amino-3-methylbutanol, 3 ml of t-butanol and 5 ml of benzene was added dropwise. After stirring at room temperature for 30 minutes, ether was added to the reaction mixture, and the solid was removed by filtration with Hyflo Super-Cel. The filtrate was concentrated under reduced pressure. n-Hexane was added to the resulting oily product, and the mixture was allowed to stand to give 2.34 g of 3-(3-amino-3-methylbutoxy)-6-chloropyridazine as colorless crystals having a melting point of 63.5° to 65.0° C.

후처리

  1. temperaturewhile being cooled with ice
  2. additionwas added dropwise
  3. stirringAfter stirring at room temperature for 30 minutes
  4. customthe solid was removed by filtration with Hyflo Super-Cel
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. additionn-Hexane was added to the resulting oily product

출처 및 근거

ORD 기록
ord-8e608fddabfc492fb74b8e5d183f2822
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599333

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