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Potassium Carbonate → HCID 10648237、化合物

HRID 617576
ノート
印刷プレビュー

反応式

HRID 617576 の反応式
[C:1]([O:4][CH2:5][CH2:6][C:7]([NH:32][C:33](=[O:35])[CH3:34])([CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23](=O)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:19][CH:18]=1)[CH2:8][CH2:9][CH2:10][O:11][C:12](=[O:14])[CH3:13])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>FC(F)(F)C(O)=O.C([SiH](CC)CC)C>[C:1]([O:4][CH2:5][CH2:6][C:7]([NH:32][C:33](=[O:35])[CH3:34])([CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:19][CH:18]=1)[CH2:8][CH2:9][CH2:10][O:11][C:12](=[O:14])[CH3:13])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 226186813-Acetamido-6-acetoxy-3-[2-(4-octanoylphenyl)ethyl]hexyl acetate

生成物 1

HCID 10648237HCID 10648237、化合物収率 64.3%

試薬・触媒・溶媒 2

HCID 6422Trifluoroacetic acid溶媒HCID 12052Triethylsilane溶媒

実験手順

To a solution of 3-acetamido-6-acetoxy-3-[2-(4-octanoylphenyl)ethyl]hexyl acetate (720 mg) in trifluoroacetic acid (15 ml), triethylsilane (0.53 ml) was added at room temperature. After stirring for an hour, the reaction solution was poured into ice-water and potassium carbonate was carefully added to the mixture to neutralize. The mixture was extracted with ethyl acetate and the extract was washed with water and a saturated brine and dried over anhydrous magnesium sulfate. The solvent was distilled away and the residue obtained was purified by silica gel chromatography (eluent; hexane-ethyl acetate=1:1) to give the subject compound (450 mg) as a colorless oily substance.

後処理

  1. additionwas carefully added to the mixture
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe extract was washed with water
  4. dry with materiala saturated brine and dried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled away
  6. customthe residue obtained
  7. customwas purified by silica gel chromatography (eluent; hexane-ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-d12ec3c6697d420eac1cdf6f86d77001
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05948820

反応ノート

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