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Acetic Acid → Propyl 5-cyano-4-(5,6-difluoro-2-methyl-4-oxo-4H-chromen-8-yl)-2,6-dimethyl-1,4-dihydropyridine-3-carboxylate

HRID 557414
ノート
印刷プレビュー

反応式

HRID 557414 の反応式
[F:1][C:2]1[C:11]([F:12])=[CH:10][C:9]([CH:13]=O)=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([CH3:15])[O:7]2.[C:17]([CH:19]=[C:20]([O-])[CH3:21])#[N:18].[Na+].[NH2:24]/[C:25](/[CH3:33])=[CH:26]\[C:27]([O:29][CH2:30][CH2:31][CH3:32])=[O:28].C(O)(=O)C>CC(O)C>[C:17]([C:19]1[CH:13]([C:9]2[CH:10]=[C:11]([F:12])[C:2]([F:1])=[C:3]3[C:8]=2[O:7][C:6]([CH3:15])=[CH:5][C:4]3=[O:16])[C:26]([C:27]([O:29][CH2:30][CH2:31][CH3:32])=[O:28])=[C:25]([CH3:33])[NH:24][C:20]=1[CH3:21])#[N:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 12706963Propyl 3-aminobut-2-enoateHCID 574388895,6-difluoro-2-methyl-4-oxo-4H-chromene-8-carbaldehydeHCID 74083625Sodium 1-cyanoprop-1-en-2-olate

生成物 1

HCID 66991482Propyl 5-cyano-4-(5,6-difluoro-2-methyl-4-oxo-4H-chromen-8-yl)-2,6-dimethyl-1,4-dihydropyridine-3-carboxylate

試薬・触媒・溶媒 1

HCID 3776
Isopropanol
溶媒

実験手順

A solution of 100 mg (0.45 mmol) of 5,6-difluoro-2-methyl-4-oxo-4H-chromene-8-carbaldehyde in 5 ml of 2-propanol is mixed with 46.9 mg (0.45 mmol) of sodium 1-cyanoprop-1-en-2-olate, 63.88 mg (0.45 mmol) of propyl 3-aminocrotonate and 0.04 ml (0.67 mmol) of acetic acid and stirred under reflux for 3 h. After cooling, the mixture is concentrated. The residue is taken up in dichloromethane and washed with water. The organic phase is dried over sodium sulfate and concentrated. The resulting residue is crystallized from diethyl ether. The beige-colored crystals are filtered off with suction and dried at 40° C. in a vacuum drying oven. 74.6 mg (40.35% of theory) of the title compound are obtained.

後処理

  1. temperatureunder reflux for 3 h
  2. temperatureAfter cooling
  3. concentrationthe mixture is concentrated
  4. washwashed with water
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. concentrationconcentrated
  7. customThe resulting residue is crystallized from diethyl ether
  8. filtrationThe beige-colored crystals are filtered off with suction
  9. customdried at 40° C. in a vacuum
  10. customdrying oven

出典と根拠

ORDレコード
ord-30b525ee7a6e4f8da4d5ba5ae3b10e86
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058447B2

反応ノート

読み込み中…

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