Ethyl cyanoacetate → HCID 54413059、化合物

HRID 1704729

反応式

HRID 1704729 の反応式
CC[O-].[Na+].[C:5]([CH2:7][C:8](OCC)=[O:9])#[N:6].[C:13]1([CH:19]=[C:20]2[C:25](=[O:26])[C:24](=[CH:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH2:23][S:22][CH2:21]2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CCO>[O:9]=[C:8]1[O:26][C:25]2[C:24](=[CH:27][C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)[CH2:23][S:22][CH2:21][C:20]=2[CH:19]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:7]1[C:5]#[N:6]

参加物

5

反応物 3

HCID 7764Ethyl cyanoacetateHCID 336779tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-oneHCID 2723922Sodium ethoxide

生成物 1

HCID 54413059HCID 54413059、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of NaOEt (from 555 mg, 92 mg atom Na in absolute EtOH) in 100 ml of absolute EtOH is added ethyl cyanoacetate (2.44 g, 22 mmole) dissolved in 50 ml of absolute EtOH. This is heated at reflux temperature for 2 hours, cooled slightly and tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-one (5.84 g, 20 mmole) is added at once. The mixture quickly turns orange-red for ca. 10 minutes, changing to yellow (yellow solids in orange-red solution) as heating is continued for 2 hours.

後処理

  1. temperatureThis is heated
  2. temperatureat reflux temperature for 2 hours
  3. temperaturecooled slightly
  4. temperatureas heating
  5. waitis continued for 2 hours

出典と根拠

ORDレコード
ord-b0cd7425e0bf47af9e85693cd6ceaf55
出典データセット
uspto-grants-1978_11
特許番号
US04127667

関連ノート

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