Sodium Acetate → HCID 20069270、化合物

HRID 982156ノート

反応式

HRID 982156 の反応式
[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]

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 67938515135861-52-8

生成物 1

HCID 20069270HCID 20069270、化合物収率 78%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a6cc4f6e102849b59953a36435580069
出典データセット
uspto-grants-1991_02
特許番号
US04994557

反応ノート

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