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

HRID 1500965ノート

反応式

HRID 1500965 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収率 80%

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% w/w, 2.2 g, 55 mmol) at −10° C. The resultant mixture was stirred for 2 hours. Then diketene (4.2 g, 50 mmol) was added dropwise to the solution. The mixture was allowed to warm to room temperature and continued stirring for 30 minutes. The mixture was neutralized with hydrochloric acid and then concentrated in vacuo to give crude 2-amino-6-methyl-4-oxo-4H-pyran-3-carbonitrile (6.0 g, 80%) as a red solid, which was used in the next step without further purification.

後処理

  1. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8d374a3dc5bb4642b70e99a071bea4d7
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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