Clofibric Acid → Clofibrate

HRID 922005

反応式

HRID 922005 の反応式
[CH3:1][C:2]([O:7][C:8]1[CH:9]=[CH:10][C:11]([Cl:14])=[CH:12][CH:13]=1)([C:4]([OH:6])=[O:5])[CH3:3].[CH3:15][C@H:16](NC)[C@H](O)C1C=CC=CC=1>>[CH3:15][CH2:16][O:5][C:4]([C:2]([O:7][C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)([CH3:1])[CH3:3])=[O:6]

参加物

3

反応物 2

HCID 2797Clofibric AcidHCID 9294Ephedrine

生成物 1

HCID 2796Clofibrate

実験手順

Clofibric acid (1.073 g, 5 mmol) and ephedrine (0.826 g, 5 mmol) were molten in a hot mortar until a free-flowing clear liquid was obtained. The mixture solidified at room temperature and was grinded to obtain a yellow powder in quantitative yield. 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=9.36 (br s, 2H), 7.30 (m, 5H), 7.19 (d, J=8.8 Hz, 2H), 6.82 (d, J=8.75 Hz, 2H), 5.10 (s, 1H), 3.12 (m, 1H), 2.52 (s, 3H), 1.41 (s, 6H), 0.85 (d, J=6.58 Hz), 3H). 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=176.8, 155.5, 141.8, 128.5, 128.0, 126.9, 125.8, 123.4, 119.2, 80.2, 69.8, 59.5, 30.7, 25.8, 9.6. mp 131° C., T5%onset 166° C.

後処理

  1. customwas obtained
  2. customsolidified at room temperature
  3. customwas grinded
  4. customto obtain a yellow powder in quantitative yield
  5. custommp 131° C., T5%onset 166° C.

出典と根拠

ORDレコード
ord-ca7d3a5197f6419f89b04ac86bf56791
出典データセット
uspto-grants-2016_03
特許番号
US09278134B2

関連ノート

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