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

HRID 925102

反応式

HRID 925102 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>[C].[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

参加物

3

反応物 1

HCID 14535936(3R)-1,1,3-trimethyl-2,3-dihydro-1H-inden-4-amine

生成物 1

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

試薬・触媒・溶媒 1

HCID 178418390HCID 178418390、化合物触媒

反応条件

温度
200 °C

実験手順

Into a reaction vessel were charged 6.00 parts by weight of (3R)-1,1,3-trimethyl-4-aminoindane (optical purity of 96.5% ee) and 1.62 parts by weight of 5% palladium-carbon (STD-type, manufactured by N. E. Chemcat Corporation), thereby obtaining a mixture. The reaction vessel was sealed, the gas in the reaction vessel was replaced with nitrogen, and then the mixture was stirred at 200° C. for 7.5 hours to obtain a reaction mixture. Thereafter, the obtained reaction mixture was cooled and filtered. The obtained solid was washed with 20 parts by weight of 2-propanol. The washing liquid recovered after washing and the filtrate obtained by filtration were combined. The combined mixture was concentrated under reduced pressure to obtain 5.06 parts by weight of 1,1,3-trimethyl-4-aminoindane. The obtained 1,1,3-trimethyl-4-aminoindane had an optical purity of 3.3% ee and a recovery rate of 84.3%.

後処理

  1. customobtaining a mixture
  2. customThe reaction vessel was sealed
  3. customto obtain a reaction mixture
  4. customThereafter, the obtained reaction mixture
  5. temperaturewas cooled
  6. filtrationfiltered
  7. washThe obtained solid was washed with 20 parts by weight of 2-propanol
  8. customThe washing liquid recovered
  9. washafter washing
  10. customthe filtrate obtained by filtration
  11. concentrationThe combined mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-44b05cb24fd24b80b36b277a428fe506
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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