Adipoyl chloride → n,n'-Bis-(1-indanyl)adipamide

HRID 650139

反応式

HRID 650139 の反応式
[NH2:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.[C:11](Cl)(=[O:19])[CH2:12][CH2:13][CH2:14][CH2:15][C:16](Cl)=[O:17]>CCOCC>[CH:2]1([NH:1][C:11](=[O:19])[CH2:12][CH2:13][CH2:14][CH2:15][C:16]([NH:1][CH:2]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[CH2:4][CH2:3]2)=[O:17])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1

参加物

4

反応物 2

HCID 61034Adipoyl chlorideHCID 123445(+-)-1-Aminoindan

生成物 1

HCID 18627800n,n'-Bis-(1-indanyl)adipamide収率 60%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

Racemic 1-aminoindan (5.7 g, 43 mmole) in ether (20 ml) stirred in ice, was treated dropwise with adipoyl chloride (1.83 g, 10 mmole) in ether (10 ml). After 30 min. the solid was filtered and slurried with water for 45 min. The insoluble solid was collected, air dried (2.82 g) and crystallized from HOAc/H2O, washed with acetic acid/water (1:1), ethanol and ether and then dried to give 2.26 g (60% title compound. Melting point: 227° C.

後処理

  1. filtrationAfter 30 min. the solid was filtered
  2. customThe insoluble solid was collected
  3. customair dried (2.82 g)
  4. customcrystallized from HOAc/H2O
  5. washwashed with acetic acid/water (1:1), ethanol and ether
  6. customdried

出典と根拠

ORDレコード
ord-7ebf826dc868480c90044b2131fbd62f
出典データセット
uspto-grants-2001_08
特許番号
US06271263B1

関連ノート

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