Dicyclohexylcarbodiimide → 4-Undecanoyloxybenzoic acid

HRID 247790

反応式

HRID 247790 の反応式
[C:1]([O:12][C:13]1[CH:43]=[CH:42][C:16]([C:17]([O:19]C2C=CC(C(OC(CCCCCCCC)C(F)(F)F)=O)=CC=2)=[O:18])=[CH:15][CH:14]=1)(=[O:11])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].O[C:45]1C=CC(C(OC(CCCCCCCC)C(F)(F)F)=O)=CC=1.C1(N=C=NC2CCCCC2)CCCCC1.CN(C1C=CC=CN=1)C>O1CCCC1>[C:1]([O:12][C:13]1[CH:14]=[CH:15][C:16]([C:17]([OH:19])=[O:18])=[CH:42][CH:43]=1)(=[O:11])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:45]

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 218852-DimethylaminopyridineHCID 147457541,1,1-Trifluoro-2-decyl 4-hydroxybenzoateHCID 190139204-(1,1,1-Trifluoro-2-decyloxycarbonyl)phenyl 4-n-decanoyloxybenzoate

生成物 1

HCID 154568744-Undecanoyloxybenzoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of the 4-undecanoyloxybenzoic acid )0.3 g) obtained in (1) above and the 1,1,1-trifluoro-2-decyl-4-hydroxybenzoate (0.3 g) obtained in Example 12, (2) in tetrahydrofuran (about 30 ml) were added dicyclohexylcarbodiimide (0.25 g) and dimethylaminopyridine (0.01 g). The mixture was stirred at room temperature for about 20 hours. The solution was distilled to remove the solvent and the residue was dissolved in dichloromethane and washed with water. The organic layer was dried over anhydrous magnesium sulfate and was distilled to remove the solvent. The residue was purified by silica-gel column chromatography (developer : hexane/ethyl acetate=20/1) to obtain the titled compound (0.21 g).

後処理

  1. distillationThe solution was distilled
  2. customto remove the solvent
  3. dissolutionthe residue was dissolved in dichloromethane
  4. washwashed with water
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. distillationwas distilled
  7. customto remove the solvent
  8. customThe residue was purified by silica-gel column chromatography (developer : hexane/ethyl acetate=20/1)

出典と根拠

ORDレコード
ord-d4f4dcd3467640efad5080b248df6aa7
出典データセット
uspto-grants-1993_05
特許番号
US05207947

関連ノート

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