Water → Methyl 6-isocyanatopyridazine-3-carboxylate

HRID 624206노트

반응식

HRID 624206 반응식
[NH2:1][C:2]1[N:7]=[N:6][C:5]([C:8]([O:10][CH3:11])=[O:9])=[CH:4][CH:3]=1.CCN(CC)CC.Cl[C:20](Cl)([O:22]C(=O)OC(Cl)(Cl)Cl)Cl.O>C1(C)C=CC=CC=1>[N:1]([C:2]1[N:7]=[N:6][C:5]([C:8]([O:10][CH3:11])=[O:9])=[CH:4][CH:3]=1)=[C:20]=[O:22]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 94429TriphosgeneHCID 14536428Methyl 6-aminopyridazine-3-carboxylate

생성물 1

HCID 86665081Methyl 6-isocyanatopyridazine-3-carboxylate

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

To the solution of methyl 6-aminopyridazine-3-carboxylate (14 g, 91.5 mmol) in anhydrous toluene (700 mL) was added Et3N (11.1, 109.8 mmol). A solution of triphosgene (27.2 g, 91.5 mmol) in anhydrous toluene was added slowly at 0° C. The reaction mixture was stirred for 2 hrs at room temperature and then heated at 90° C. for 5 hrs. After cooling to room temperature, toluene and water were added to the mixture, the mixture was separated and the organic layer was dried over anhydrous Na2SO4, concentrated under reduced pressure to give the title compound as a solid.

후처리

  1. temperatureheated at 90° C. for 5 hrs
  2. temperatureAfter cooling to room temperature
  3. customthe mixture was separated
  4. dry with materialthe organic layer was dried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f9df310a43324073963e6c71e30a482f
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302989B2

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