Water → Methyl 6-isocyanatopyridazine-3-carboxylate

HRID 624206ノート

反応式

HRID 624206 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 86665081Methyl 6-isocyanatopyridazine-3-carboxylate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f9df310a43324073963e6c71e30a482f
出典データセット
uspto-grants-2016_04
特許番号
US09302989B2

反応ノート

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