3-(2-Amino-2-methylpropoxy)-6-chloropyridazine → 1-(2-Chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol

HRID 745494노트

반응식

HRID 745494 반응식
[NH2:1][C:2]([CH3:13])([CH3:12])[CH2:3][O:4][C:5]1[N:6]=[N:7][C:8]([Cl:11])=[CH:9][CH:10]=1.[Cl:14][C:15]1[C:25]([CH3:26])=[CH:24][CH:23]=[CH:22][C:16]=1[O:17][CH2:18][CH:19]1[O:21][CH2:20]1>CO>[Cl:14][C:15]1[C:25]([CH3:26])=[CH:24][CH:23]=[CH:22][C:16]=1[O:17][CH2:18][CH:19]([OH:21])[CH2:20][NH:1][C:2]([CH3:13])([CH3:12])[CH2:3][O:4][C:5]1[N:6]=[N:7][C:8]([Cl:11])=[CH:9][CH:10]=1

참가 물질

4

반응물 2

HCID 103304683-(2-Amino-2-methylpropoxy)-6-chloropyridazineHCID 233133352-[(2-Chloro-3-methylphenoxy)methyl]oxirane

생성물 1

HCID 99783091-(2-Chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol수율 66.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 6.04 g of 3-(2-amino-2-methylpropoxy)-6-chloropyridazine obtained in Example 1, (a) and 5.95 g of 1-(2-chloro-3-methylphenoxy)-2,3-epoxypropane in 120 ml of methanol was refluxed for 3 hours. The solvent was evaporated under reduced pressure. A solution of the residue in benzene was extracted with 175 ml of 0.2N hydrochloric acid. The aqueous layer was made alkaline with potassium carbonate and extracted with chloroform. The chloroform layer was dried over sodium sulfate. The solvent was evaporated and the residue (10 g) was purified by column chromatography (50 g of Florisil; eluted with chloroform) to give 7.98 g of 1-(2-chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol as a colorless oil.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. extractionA solution of the residue in benzene was extracted with 175 ml of 0.2N hydrochloric acid
  3. extractionextracted with chloroform
  4. dry with materialThe chloroform layer was dried over sodium sulfate
  5. customThe solvent was evaporated
  6. customthe residue (10 g) was purified by column chromatography (50 g of Florisil; eluted with chloroform)

출처 및 근거

ORD 기록
ord-d970a2615e1946218829aff55aee5dab
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599333

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