Sodium Acetate → HCID 20069270, 화합물

HRID 982156노트

반응식

HRID 982156 반응식
[CH2:1]([Sn:5]([CH2:24][CH2:25][CH2:26][CH3:27])([CH2:20][CH2:21][CH2:22][CH3:23])[C:6]1[CH:7]=[C:8]([NH:12][C:13](=[O:19])/[CH:14]=[CH:15]\[C:16](O)=[O:17])[CH:9]=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH3:4].C([O-])(=O)C.[Na+]>C(OC(=O)C)(=O)C>[CH2:1]([Sn:5]([CH2:20][CH2:21][CH2:22][CH3:23])([CH2:24][CH2:25][CH2:26][CH3:27])[C:6]1[CH:7]=[C:8]([N:12]2[C:16](=[O:17])[CH:15]=[CH:14][C:13]2=[O:19])[CH:9]=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 67938515135861-52-8

생성물 1

HCID 20069270HCID 20069270, 화합물수율 78%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

N-(m tri-n butylstannylphenyl)maleamic acid prepared as described above (0.40 g, 0.83 mmol) was placed in acetic anhydride (6 mL). Sodium acetate (0.43 g) was added and the solution stirred for 15 minutes at room temperature. After the reaction became homogeneous, the reaction mixture was stirred for 3 hours at 120° C. The filtrate obtained from this brown mixture was evaporated to dryness under reduced pressure and the residue was dissolved in ethyl ether. The ether mixture was filtered and the filtrate was again evaporated to dryness The compound was obtained by flash chromatography on a 30×200 mm column of Kieselgel 60, 230-400 mesh, eluted with ethyl acetate/hexane (1:5) (100 mL) to yield ten fractions. Fractions 6-9 were combined to give the desired product as an orange oil (0.3, 78%): TLC (EtOAc/hexane, 1:5) Rf 0.30; 1H NMR (CDCl3), δ); 7.3-7.5 (multiplets, 4H, 4 aryl CH); 6.8 (singlet, 2H, 2 CHC=O); 0.9-1.6 (multiplets, 27H, 3×n-C4H9).

후처리

  1. stirringthe reaction mixture was stirred for 3 hours at 120° C
  2. customThe filtrate obtained from this brown mixture
  3. customwas evaporated to dryness under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl ether
  5. filtrationThe ether mixture was filtered
  6. customthe filtrate was again evaporated to dryness The compound
  7. customwas obtained by flash chromatography on a 30×200 mm column of Kieselgel 60, 230-400 mesh
  8. washeluted with ethyl acetate/hexane (1:5) (100 mL)
  9. customto yield ten fractions

출처 및 근거

ORD 기록
ord-a6cc4f6e102849b59953a36435580069
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04994557

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