Potassium Hydroxide → HCID 21423155、化合物

HRID 2397279ノート

反応式

HRID 2397279 の反応式
[Cl-:1].[Al+3].[Cl-].[Cl-].[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:11]([CH2:13][CH2:14][CH:15]1[CH2:24][C:23]2[CH:22]([O:25][CH3:26])[N:21]([O:27][CH3:28])[CH:20]=[C:19]3[O:29][CH2:30][CH2:31][CH:17]([C:18]=23)[CH2:16]1)#[N:12].[OH-].[K+]>CCOCC.O1CCCC1.O>[ClH:1].[ClH:1].[NH2:12][CH2:11][CH2:13][CH2:14][CH:15]1[CH2:24][C:23]2[CH:22]([O:25][CH3:26])[N:21]([O:27][CH3:28])[CH:20]=[C:19]3[O:29][CH2:30][CH2:31][CH:17]([C:18]=23)[CH2:16]1

参加物

8

反応物 4

HCID 14797Potassium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 21226445Aluminium lithium hydrideHCID 70631280HCID 70631280、化合物

生成物 1

HCID 21423155HCID 21423155、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒3 回HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of aluminum chloride (5.6 g) in anhydrous ether (80 ml) is added dropwise to a stirred suspension of lithium aluminum hydride (1.6 g) in anhydrous ether (80 ml). The mixture is stirred at room temperature for 0.5 hr. and then a solution of the nitrile, 5-cyanoethyl-1,2,3a,4,5,6-hexahydro-7,8-dimethoxypyrano[2,3,4-de]isoquinoline (7 g), described in Example 61, in anhydrous ether (100 ml) is added dropwise during 2 hr. The mixture is heated under reflux for 2 hr. and then cooled (ice bath) and a solution of water (12 ml) in tetrahydrofuran (60 ml) is added. The mixture is heated under reflux for 15 minutes, cooled and water (20 ml) is added, followed by 10% KOH solution until the aqueous phase is rendered basic. The mixture is filtered, washing well with ether. the ether solution is collected and the aqueous phase is saturated with salt and extracted with chloroform. The organic solutions are combined and evaporated to yield the title compound, λmaxEtOH 284 nm (1830). max

後処理

  1. additionis added dropwise during 2 hr
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 2 hr
  4. temperatureand then cooled (ice bath)
  5. temperatureThe mixture is heated
  6. temperatureunder reflux for 15 minutes
  7. temperaturecooled
  8. filtrationThe mixture is filtered
  9. washwashing well with ether
  10. customthe ether solution is collected
  11. extractionextracted with chloroform
  12. customevaporated

出典と根拠

ORDレコード
ord-210ce89a9c214af6aea5cf5386da888e
出典データセット
uspto-grants-1977_05
特許番号
US04021451

反応ノート

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