(3R)-1,1,3-trimethyl-2,3-dihydro-1H-inden-4-amine → 1,1,3-Trimethylindan-4-amine

HRID 925106

반응식

HRID 925106 반응식
[CH3:1][C:2]1([CH3:13])[C:10]2[C:5](=[C:6]([NH2:11])[CH:7]=[CH:8][CH:9]=2)[C@H:4]([CH3:12])[CH2:3]1.[H][H]>C1(C)C=CC=CC=1.[Pd]>[CH3:1][C:2]1([CH3:13])[C:10]2[C:5](=[C:6]([NH2:11])[CH:7]=[CH:8][CH:9]=2)[CH:4]([CH3:12])[CH2:3]1

참가 물질

5

반응물 2

HCID 14535936(3R)-1,1,3-trimethyl-2,3-dihydro-1H-inden-4-amineHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 112175411,1,3-Trimethylindan-4-amine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 1140Toluene용매

실험 절차

Into a reaction vessel were charged 31.2 parts by weight of (3R)-1,1,3-trimethyl-4-aminoindane (optical purity of 67.0% ee) and 0.83 part by weight of 4.5% palladium-0.5% platinum-carbon (ASCA-2, manufactured by N. E. Chemcat Corporation), thereby obtaining a mixture. The reaction vessel was sealed and the gas in the reaction vessel was replaced with nitrogen. While the mixture was stirred, into the reaction vessel was charged hydrogen until the internal pressure of hydrogen in the reaction vessel reached 0.5 MPa, and the mixture was stirred at an internal temperature of 60° C. After 1 hour, the gas in the reaction vessel was replaced with nitrogen, and the mixture was stirred at an internal temperature of 180° C. and an internal pressure of 0.3 MPa for 12.5 hours, thereby obtaining a reaction mixture. The obtained reaction mixture was cooled and filtered. The obtained solid was washed with 45 parts by weight of toluene. The washing liquid recovered after washing and the filtrate obtained by filtration were combined to obtain a solution of 77.5 parts by weight of 1,1,3-trimethyl-4-aminoindane in toluene. The combined 1,1,3-trimethyl-4-aminoindane had an optical purity of 0.29% ee and a recovery rate of 97.7%.

후처리

  1. customobtaining a mixture
  2. customThe reaction vessel was sealed
  3. stirringthe mixture was stirred at an internal temperature of 60° C
  4. stirringthe mixture was stirred at an internal temperature of 180° C.
  5. waitan internal pressure of 0.3 MPa for 12.5 hours
  6. customobtaining a reaction mixture
  7. customThe obtained reaction mixture
  8. temperaturewas cooled
  9. filtrationfiltered
  10. washThe obtained solid was washed with 45 parts by weight of toluene
  11. customThe washing liquid recovered
  12. washafter washing
  13. customthe filtrate obtained by filtration

출처 및 근거

ORD 기록
ord-a80aaf3b54864250ba606372f470ef1e
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09284260B2

연결된 노트

불러오는 중…