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

HRID 925104

反応式

HRID 925104 の反応式
[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>[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

参加物

4

反応物 2

HCID 14535936(3R)-1,1,3-trimethyl-2,3-dihydro-1H-inden-4-amineHCID 178418361HCID 178418361、化合物2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Into a reaction vessel were charged 31.7 parts by weight of (3R)-1,1,3-trimethyl-4-aminoindane (optical purity of 67.0% ee) and 0.36 parts by weight of 5% palladium-alumina, 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 155° C. and an internal pressure of 0.1 MPa for 7 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 73.4 parts by weight of 1,1,3-trimethyl-4-aminoindane in toluene. The obtained 1,1,3-trimethyl-4-aminoindane had an optical purity of 4.5% ee and a recovery rate of 98.7%.

後処理

  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 155° C.
  5. waitan internal pressure of 0.1 MPa for 7 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

出典と根拠

ORDレコード
ord-edba83fe96da4a5984f91996630b1b44
出典データセット
uspto-grants-2016_03
特許番号
US09284260B2

関連ノート

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