Acetonitrile → 2-Cyano-5-(3-phenoxypropoxy)indan-1,3-dione

HRID 2050169

반응식

HRID 2050169 반응식
[O:1]([CH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:13]=[C:14]([C:22]([O:24]C)=O)[C:15](=[CH:20][CH:21]=1)[C:16]([O:18]C)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:26](#[N:28])[CH3:27].[H-].[Na+]>CCOCC>[C:26]([CH:27]1[C:22](=[O:24])[C:14]2[C:15](=[CH:20][CH:21]=[C:12]([O:11][CH2:10][CH2:9][CH2:8][O:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH:13]=2)[C:16]1=[O:18])#[N:28]

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 24758Sodium hydrideHCID 20331397Dimethyl 4-(3-phenoxypropoxy)phthalate

생성물 1

HCID 203314172-Cyano-5-(3-phenoxypropoxy)indan-1,3-dione수율 86%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of dimethyl 4-(3-phenoxypropoxy)phthalate (6.5 g; 0.019 mole), acetonitrile (10ml) and sodium hydride (0.69 g of 100%) was stirred at 100° for 6 hours and dry ether added to the cooled yellow product. The solid which separated was filtered off, dissolved in water and the solution strongly acidified with concentrated hydrochloric acid. Filtration of the precipitated solid gave the title compound which recrystallised from ethanol dilute hydrochloric acid with mp 148°-150° (dec) and in 86% yield. (Found; C, 69.00; H, 4.90; N, 4.41; C19H15NO4 0.5 H2O requires; C, 69.08; H, 4.88; N, 4.24%).

후처리

  1. customThe solid which separated
  2. filtrationwas filtered off
  3. dissolutiondissolved in water
  4. filtrationFiltration of the precipitated solid

출처 및 근거

ORD 기록
ord-75fc97bce77844d9bcc2a986a0fd8439
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04200577

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