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

HRID 650139

반응식

HRID 650139 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7ebf826dc868480c90044b2131fbd62f
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271263B1

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