Hydrochloric Acid → 1-n-Butylamino-4,6-dimethyl-7-hydroxyindane hydrochloride

HRID 414693

반응식

HRID 414693 반응식
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[C:7]2[C:3]=1[CH2:4][CH2:5][C:6]2=O.[CH2:14]([NH2:18])[CH2:15][CH2:16][CH3:17].[BH4-].[Na+].[ClH:21].C([O-])(=O)C.[Na+]>O.C(O)C>[ClH:21].[CH2:14]([NH:18][CH:6]1[C:7]2[C:3](=[C:2]([CH3:1])[CH:10]=[C:9]([CH3:11])[C:8]=2[OH:12])[CH2:4][CH2:5]1)[CH2:15][CH2:16][CH3:17]

참가 물질

8

반응물 5

HCID 313Hydrochloric Acid3회HCID 8007ButylamineHCID 2407184,6-Dimethyl-7-hydroxy-1-indanoneHCID 517045Sodium AcetateHCID 4311764Sodium borohydride

생성물 1

HCID 136042031-n-Butylamino-4,6-dimethyl-7-hydroxyindane hydrochloride

시약·촉매·용매 2

HCID 702Ethanol용매3회HCID 962Water용매

실험 절차

100 Milliliters of ethanol solution containing 1.76 g of 4,6-dimethyl-7-hydroxy-1-indanone and 14.6 g of n-butylamine was refluxed by heating for 8 hours. The reaction mixture was cooled to a room temperature, then 1.0 g of sodium borohydride was added thereto. The mixture was further stirred at a room temperature for 1 hour. The reaction mixture was concentrated to dryness and the residue obtained was dissolved in 100 ml of water. Then the solution was acidified by adding a concentrated hydrochloric acid, and the pH of the solution was adjusted to about pH=9 by adding a saturated sodium acetate aqueous solution. The precipitate formed was extracted with ethyl acetate, washed with water and dried. The solvent was removed by evaporation, the residue obtained was dissolved in 100 ml of ethanol, and changed to hydrochloride by adding ethanol being saturated with hydrogen chloride gas. Recrystallized from ethanol-ether to obtain 1.89 g of 1-n-butylamino-4,6-dimethyl-7-hydroxyindane hydrochloride in the form of colorless needle-liee crystals. Melting point: 143°-144° C.

후처리

  1. temperaturewas refluxed
  2. temperatureby heating for 8 hours
  3. concentrationThe reaction mixture was concentrated to dryness
  4. customthe residue obtained
  5. customThe precipitate formed
  6. extractionwas extracted with ethyl acetate
  7. washwashed with water
  8. customdried
  9. customThe solvent was removed by evaporation
  10. customthe residue obtained
  11. customRecrystallized from ethanol-ether

출처 및 근거

ORD 기록
ord-a57bc510ba94475d92c3cf9b77a8736b
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792628

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