Hydrochloric Acid → HCID 71607581、化合物

HRID 714493

反応式

HRID 714493 の反応式
[CH:1]1[C:6]([C@@H:7]2[O:16][C:15]3[CH:14]=[C:13]([OH:17])[CH:12]=[C:11]([OH:18])[C:10]=3[CH2:9][C@@H:8]2[OH:19])=[CH:5][C:4]([OH:20])=[C:3]([OH:21])[CH:2]=1.[C:22](OC(=O)C)(=[O:24])[CH3:23].N1[CH:34]=[CH:33]C=CC=1.Cl.CN(C=[O:40])C>>[C:22]([O:21][C:3]1[CH:2]=[CH:1][C:6]([C@@H:7]2[C@H:8]([OH:19])[CH2:9][C:10]3[C:15](=[CH:14][C:13]([OH:17])=[CH:12][C:11]=3[OH:18])[O:16]2)=[CH:5][C:4]=1[O:20][C:33](=[O:40])[CH3:34])(=[O:24])[CH3:23]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 182232(+)-Epicatechin

生成物 1

HCID 71607581HCID 71607581、化合物

実験手順

To a stirred solution of (±) epicatechin 1 (0.10 gm, 0.34 mmol) in DMF, Acetic anhydride (0.11 ml, 0.10 mmol) and pyridine (0.08 ml, 0.10 mmol) was added at room temperature. After an additional stirring at this for 24 h, 2N HCl was added and extracted with ethyl acetate (2×50 ml). The combined organic layer was washed with brine and dried over sodium sulphate. The crude reaction mixture was purified using preparative HPLC to afford 4-((2R,3R)-3,5,7-trihydroxychroman-2-yl)-1,2-phenylene diacetate (0.004 gm) and 4-((2R,3R)-3,5,7-trihydroxychroman-2-yl)-1,2-phenylene diacetate (0.008 gm) as a white solid material.

後処理

  1. extractionextracted with ethyl acetate (2×50 ml)
  2. washThe combined organic layer was washed with brine
  3. dry with materialdried over sodium sulphate
  4. customThe crude reaction mixture
  5. customwas purified

出典と根拠

ORDレコード
ord-48edf0783c39400e824884187be41586
出典データセット
uspto-grants-2015_11
特許番号
US09187448B2

関連ノート

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