Water → 4-Pyridazinecarbonitrile, 3-((2-(4-morpholinyl)ethyl)amino)-6-phenyl-, dihydrochloride

HRID 1249356노트

반응식

HRID 1249356 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][C:7]=1[C:8]#[N:9].[NH2:16][CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.O>C(O)CCC>[ClH:1].[ClH:1].[O:22]1[CH2:23][CH2:24][N:19]([CH2:18][CH2:17][NH:16][C:2]2[N:3]=[N:4][C:5]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[CH:6][C:7]=2[C:8]#[N:9])[CH2:20][CH2:21]1

참가 물질

5

반응물 3

HCID 962WaterHCID 4082852-MorpholinoethylamineHCID 6404487HCID 6404487, 화합물

생성물 1

HCID 30232604-Pyridazinecarbonitrile, 3-((2-(4-morpholinyl)ethyl)amino)-6-phenyl-, dihydrochloride수율 81.3%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

7.3 g of the chlorine compound of Example 18 are dissolved in 60 ml of normal butanol, and 8 g of N-(2-aminoethyl)-morpholine are added. The mixture is heated under reflux for 3 hours and then poured into 1000 ml of water. The organic phase is extracted with ether and the ether solution is then extracted with a 1N solution of sulphuric acid. The aqueous phase is separated off, rendered alkaline with sodium hydroxide and extracted with ether. The ether phase is dried over magnesium sulphate and the solvent is then evaporated off to dryness in vacuo. This gives a yellow solid. Yield 81.3%; melting point 138° C.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. extractionThe organic phase is extracted with ether
  4. extractionthe ether solution is then extracted with a 1N solution of sulphuric acid
  5. customThe aqueous phase is separated off
  6. extractionextracted with ether
  7. dry with materialThe ether phase is dried over magnesium sulphate
  8. customthe solvent is then evaporated off to dryness in vacuo
  9. customThis gives a yellow solid

출처 및 근거

ORD 기록
ord-ad55efd06a7942e38586ede1ba1dc52b
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04631280

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