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Diclofenac → 4-Carbamoylphenyl 2-[2-(2,6-dichlorophenylamino)-phenyl]acetate

HRID 18626
ノート
印刷プレビュー

反応式

HRID 18626 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]([NH:11][C:12]2[C:13]([Cl:19])=[CH:14][CH:15]=[CH:16][C:17]=2[Cl:18])=[C:5]([CH2:7][C:8]([OH:10])=[O:9])[CH:6]=1.OC1C2N=NNC=2C=CC=1.C1CCC(N=C=NC2CCCCC2)CC1.O[C:46]1[CH:54]=[CH:53][C:49]([C:50]([NH2:52])=[O:51])=[CH:48][CH:47]=1>CN(C)C=O.C(Cl)(Cl)Cl>[Cl:19][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]([Cl:18])[C:12]=1[NH:11][C:4]1[CH:3]=[CH:2][CH:1]=[CH:6][C:5]=1[CH2:7][C:8]([O:10][C:46]1[CH:54]=[CH:53][C:49]([C:50](=[O:51])[NH2:52])=[CH:48][CH:47]=1)=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 3033DiclofenacHCID 10868DicyclohexylcarbodiimideHCID 650524-HydroxybenzamideHCID 178418300HCID 178418300、化合物

生成物 1

HCID 593455914-Carbamoylphenyl 2-[2-(2,6-dichlorophenylamino)-phenyl]acetate収率 17%

試薬・触媒・溶媒 2

HCID 6212
Chloroform
溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

To the solution of 1 (diclofenac, 890 mg, 3.0 mmol) in 50 mL of N,N-dimethylformamide, hydroxybenzotriazole (445 mg, 3.3 mmol) and DCC (680 mg, 3.3 mmol) were added with stirring at 0° C. for 1 h. To the reaction mixture 4-hydroxybenzamide (4, 616 mg, 4.5 mmol) was added and stirred for 1 h at 0° C. and 3 hs at room temperature. After filtration, the filtrate was evaporated under reduced pressure and the oily residue thus obtained was dissolved in chloroform; the organic layer was washed with brine, dried on anhydrous MgSO4, filtered and the solvent evaporated. The crude product 5 was loaded on a silica gel open column and eluted with CH2Cl2/MeOH (9/1), from which 4-carbamoylphenyl 2-(2-(2,6-dichlorophenylamino)phenyl)acetate (5) was obtained (212 mg, 17% yield).

後処理

  1. stirringstirred for 1 h at 0° C.
  2. customat room temperature
  3. filtrationAfter filtration
  4. customthe filtrate was evaporated under reduced pressure
  5. customthe oily residue thus obtained
  6. washthe organic layer was washed with brine
  7. dry with materialdried on anhydrous MgSO4
  8. filtrationfiltered
  9. customthe solvent evaporated
  10. washeluted with CH2Cl2/MeOH (9/1), from which 4-carbamoylphenyl 2-(2-(2,6-dichlorophenylamino)phenyl)acetate (5)
  11. customwas obtained (212 mg, 17% yield)

出典と根拠

ORDレコード
ord-efdd765be6a748e18147c7442f20519c
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07741359B2

反応ノート

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