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Dimethylformamide → HCID 54508018、化合物

HRID 1602510
ノート
印刷プレビュー

反応式

HRID 1602510 の反応式
Br[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[S:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[CH:17]=[CH:18][C:19]1[CH:47]=[CH:46][C:22]([C:23]([NH:25][C:26]2[CH:31]=[C:30]([CH2:32][CH2:33][CH2:34][S:35]([C:38]3[CH:43]=[CH:42][C:41]([Cl:44])=[CH:40][CH:39]=3)(=[O:37])=[O:36])[CH:29]=[CH:28][C:27]=2[OH:45])=[O:24])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[S:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[CH:17]=[CH:18][C:19]1[CH:47]=[CH:46][C:22]([C:23]([NH:25][C:26]2[CH:31]=[C:30]([CH2:32][CH2:33][CH2:34][S:35]([C:38]3[CH:39]=[CH:40][C:41]([Cl:44])=[CH:42][CH:43]=3)(=[O:37])=[O:36])[CH:29]=[CH:28][C:27]=2[O:45][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:24])=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 53752128HCID 53752128、化合物

生成物 1

HCID 54508018HCID 54508018、化合物収率 62%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Under ice-cooling, ethyl bromoacetate (87 mg, 0.52 mmol) was added dropwise to a mixture of 4-[2-(2-benzothiazolyl)vinyl]-5'-[3-(4-chlorophenylsulfonyl)propyl]-2'-hydroxybenzanilide (307 mg, 0.52 mmol), potassium carbonate (145 mg, 1.05 mmol) and dimethylformamide (10 ml), and the resulting reaction solution was stirred at room temperature for 12 hours. Water was added to the reaction solution and the product formed was extracted with ethyl acetate. The resulting extract was washed with water and brine in that order, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. Thereafter, the resulting residue was purified by silica gel column chromatography (eluent=hexane:ethyl acetate=4:1) to give ethyl 2-[4-[2-(2-benzothiazolyl)vinyl]benzoylamino]-4-[3-(4-chlorophenylsulfonyl)propyl]phenoxyacetate (219 mg, 0.32 mmol, 62%) as colorless solid.

後処理

  1. temperatureUnder ice-cooling
  2. customthe resulting reaction solution
  3. customthe product formed
  4. extractionwas extracted with ethyl acetate
  5. extractionThe resulting extract
  6. washwas washed with water and brine in that order
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThereafter, the resulting residue was purified by silica gel column chromatography (eluent=hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-c45d15a5c0c34457a0b10bf4cf5be80f
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05981559

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート