Potassium Hydroxide → HCID 21423155, 화합물

HRID 259117노트

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HRID 259117 반응식
[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

참가 물질

8

반응물 4

HCID 14797Potassium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 21226445Aluminium lithium hydrideHCID 70631280HCID 70631280, 화합물

생성물 1

HCID 21423155HCID 21423155, 화합물

시약·촉매·용매 3

HCID 962Water용매2회HCID 3283Diethyl Ether용매3회HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7606d95e6e4547c493519878476e2c4e
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036842

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