Hydrochloric Acid → HCID 18182605、化合物

HRID 1264216ノート

反応式

HRID 1264216 の反応式
C[O:2][C:3](=[O:18])[C:4]([C:7]1[CH:12]=[CH:11][C:10]([C:13]2[O:14][CH:15]=[CH:16][CH:17]=2)=[CH:9][CH:8]=1)([CH3:6])[CH3:5].[OH-].[Na+].Cl>CO.C1COCC1.CCOCC>[O:14]1[CH:15]=[CH:16][CH:17]=[C:13]1[C:10]1[CH:11]=[CH:12][C:7]([C:4]([CH3:6])([CH3:5])[C:3]([OH:18])=[O:2])=[CH:8][CH:9]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21350305HCID 21350305、化合物

生成物 1

HCID 18182605HCID 18182605、化合物収率 94.3%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 21899815MeOH tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

To a solution of 2-(4-(furan-2-yl)-phenyl)-2-methyl-propionic acid methyl ester (2.0 g, 8.2 mmol) (reference example 30a) in MeOH/THF (20 mL, 1/1) is added NaOH (2 mL, 6M). The resulting solution is stirred for 1 hour then heated to 65° C. and stirred at this temperature for 2 hours. The reaction mixture is then cooled and acidified (to pH 1) with hydrochloric acid (2 M). The resulting mixture is diluted with ether, washed with water and brine, dried over MgSO4 and concentrated to give 1.78 g of the title compound as a solid. 1H NMR (CDCl3) d 1.61 (s, 6H), 6.45 (dd, J 3, 2 Hz, 1H), 6.62 (d, J=3 Hz, 1H), 7.42 (m, 2H), 7.45 (d, J=2 Hz, 1H), 7.64 (m, 2H). MS (EI) m/z 230 (M+)

後処理

  1. stirringstirred at this temperature for 2 hours
  2. temperatureThe reaction mixture is then cooled
  3. washwashed with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-e5dc483d59ff42a4b9e6ce97da87d3e7
出典データセット
uspto-grants-2003_04
特許番号
US06541505B1

反応ノート

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