4,4'-Diazenediyldianiline → N-Boc-pyrrolidine

HRID 79771

반응식

HRID 79771 반응식
NC1C=CC(N=NC2C=CC(N)=CC=2)=CC=1.[C:17]([O:21][C:22]([N:24]1[CH2:28][CH2:27][CH2:26][CH:25]1C(O)=O)=[O:23])([CH3:20])([CH3:19])[CH3:18].C(OC(N1C2C(=CC=CC=2)C=CC1)=O)C>C(Cl)Cl>[C:17]([O:21][C:22]([N:24]1[CH2:28][CH2:27][CH2:26][CH2:25]1)=[O:23])([CH3:20])([CH3:18])[CH3:19]

참가 물질

5

반응물 3

HCID 108554,4'-DiazenediyldianilineHCID 278131(2H)-Quinolinecarboxylic acid, ethyl esterHCID 2684721-[(Tert-butoxy)carbonyl]pyrrolidine-2-carboxylic acid

생성물 1

HCID 643455N-Boc-pyrrolidine수율 166.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-(4-aminophenylazo)-phenylamine (3.02 g) and pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester (7.00 g) were dissolved in DCM (90 mL), and 1-ethoxycarbonyl-1,2-dihydroquinoline (8.45 g) was added. The reaction mixture was stirred at ambient temperature for 19 hours and evaporated under vacuum. Oil was dissolved in ethyl acetate, forming a precipitate, which was collected by vacuum filtration and dried under vacuum, giving 2-(4-{4-[(1-carboxylic acid tert-butyl ester-pyrrolidine-2-carbonyl)-amino]-phenylazo}-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (9.28 g) as a brown solid.

후처리

  1. customevaporated under vacuum
  2. dissolutionOil was dissolved in ethyl acetate
  3. customforming a precipitate, which
  4. filtrationwas collected by vacuum filtration
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-a4efa86890aa4b198e2f4732a94ed2eb
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841278B2

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