Pyridine → 4-(4-t-Butylazo-4-cyanopentoxycarbonyl)phthalic Anhydride

HRID 866733

반응식

HRID 866733 반응식
Cl[C:2]([C:4]1[CH:5]=[C:6]2[C:11](=[O:12])[O:10][C:8](=[O:9])[C:7]2=[CH:13][CH:14]=1)=[O:3].[C:15]([N:19]=[N:20][C:21]([C:27]#[N:28])([CH2:23][CH2:24][CH2:25][OH:26])[CH3:22])([CH3:18])([CH3:17])[CH3:16].N1C=CC=CC=1>CCOCC>[C:15]([N:19]=[N:20][C:21]([C:27]#[N:28])([CH3:22])[CH2:23][CH2:24][CH2:25][O:26][C:2]([C:4]1[CH:5]=[C:6]2[C:11](=[O:12])[O:10][C:8](=[O:9])[C:7]2=[CH:13][CH:14]=1)=[O:3])([CH3:18])([CH3:16])[CH3:17]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 70998Trimellitic anhydride chlorideHCID 233458984-t-Butylazo-4-cyanopentanol

생성물 1

HCID 543368904-(4-t-Butylazo-4-cyanopentoxycarbonyl)phthalic Anhydride

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 2.1 g. (0.01 m) of 4-chloroformylphthalic anhydride in 25 ml ether in a 50 ml 4-neck round bottom flask equipped with a condenser containing a CaCl2 drying tube, a thermometer, a magnetic stirring bar and a dropping funnel was added a solution of 2.0 g. (0.01 m) 2-t-butylazo-2-cyano-5-hydroxypentane (from XIV) and 0.8 g. (0.01 m) pyridine in 10 ml ether. This solution was added dropwise with stirring over 15 minutes holding the temperature between 15° and 22° C with a water bath. The reaction was stirred an additional hour after the addition was completed and the pyridine hydrochloride filtered off. The ether filtrate was dried over anhydrous Na2SO4, filtered and evaporated to dryness leaving 3.1 g. (84%) of a viscous liquid. The infrared spectrum contained 3 carbonyl bands and no OH bands.

후처리

  1. additioncontaining a CaCl2 drying tube
  2. additiona thermometer, a magnetic stirring bar and a dropping funnel was added a solution of 2.0 g
  3. additionThis solution was added dropwise
  4. customthe temperature between 15° and 22° C
  5. stirringThe reaction was stirred an additional hour
  6. additionafter the addition
  7. filtrationthe pyridine hydrochloride filtered off
  8. dry with materialThe ether filtrate was dried over anhydrous Na2SO4
  9. filtrationfiltered
  10. customevaporated to dryness
  11. customleaving 3.1 g

출처 및 근거

ORD 기록
ord-0f9f4886c6584476adc3a7e77079ba51
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04101522

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