ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 925103
ノート
印刷プレビュー

反応式

HRID 925103 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]>[C].[Pd].CC(O)C>[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

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 2

HCID 178418390HCID 178418390、化合物触媒HCID 3776Isopropanol溶媒

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), 0.81 part by weight of 5% palladium-carbon (STD-type, manufactured by N. E. Chemcat Corporation), and 12 parts by weight of 2-propanol, thereby obtaining a mixture. The reaction vessel was sealed and the gas in the reaction vessel was replaced with nitrogen. While stirring the mixture at room temperature, into the reaction vessel was charged hydrogen until the internal pressure of hydrogen in the reaction vessel reached 0.5 MPa. After 15 minutes, hydrogen was removed to normal pressure, and the mixture was stirred at an internal temperature of 130° C. and an internal pressure of 0.45 MPa for 7 hours while the inside of the reaction vessel was replaced with hydrogen, thereby obtaining a reaction mixture. 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 5.55 parts by weight of 1,1,3-trimethyl-4-aminoindane. The obtained 1,1,3-trimethyl-4-aminoindane had an optical purity of 1.2% ee and a recovery rate of 92.5%.

後処理

  1. customobtaining a mixture
  2. customThe reaction vessel was sealed
  3. customhydrogen was removed to normal pressure
  4. stirringthe mixture was stirred at an internal temperature of 130° C.
  5. waitan internal pressure of 0.45 MPa for 7 hours while the inside of the reaction vessel was replaced with hydrogen
  6. customobtaining a reaction mixture
  7. customThe obtained reaction mixture
  8. temperaturewas cooled
  9. filtrationfiltered
  10. washThe obtained solid was washed with 20 parts by weight of 2-propanol
  11. customThe washing liquid recovered
  12. washafter washing
  13. customthe filtrate obtained by filtration
  14. concentrationThe combined mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-7a20845646eb4a0fa20b237c9745d601
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09284260B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート