Hydrochloric Acid → 2-Amino-6-methyl-4-oxo-4H-pyran-3-carbonitrile

HRID 1501259ノート

反応式

HRID 1501259 の反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[H-].[Na+].[CH2:8]=[C:9]1[O:13][C:11](=[O:12])[CH2:10]1.Cl>O1CCCC1>[NH2:4][C:3]1[O:13][C:9]([CH3:8])=[CH:10][C:11](=[O:12])[C:2]=1[C:1]#[N:5]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8010MalononitrileHCID 12661DiketeneHCID 24758Sodium hydride

生成物 1

HCID 114805352-Amino-6-methyl-4-oxo-4H-pyran-3-carbonitrile

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of malononitrile (3.3 g, 50 mmol) in anhydrous tetrahydrofuran (100 mL) was added sodium hydride (60%, 2.2 g, 55 mmol) at −10° C. The resulting reaction mixture was stirred for 2 hours. Then diketene (4.2 g, 50 mmol) was added dropwise to the solution. The reaction mixture was allowed to warmed to room temperature and continued to stir for 30 minutes. The mixture was neutralized with hydrochloric acid, and then concentrated in vacuo to give crude product as red solid, which was used in the next step without further purification.

後処理

  1. customThe resulting reaction mixture
  2. stirringto stir for 30 minutes
  3. concentrationconcentrated in vacuo
  4. customto give crude product as red solid, which
  5. customwas used in the next step without further purification

出典と根拠

ORDレコード
ord-6375d35d2162482288e00c0bda8fb246
出典データセット
uspto-grants-2015_12
特許番号
US09206128B2

反応ノート

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