Methanol → HCID 23665160、化合物

HRID 322957

反応式

HRID 322957 の反応式
[OH:1][CH:2]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:18])[CH2:3][CH2:4][C:5]([O:7]C(C)(C)C)=[O:6].CO.[OH-].[Na+:22]>O1CCCC1>[OH:1][CH:2]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:18])[CH2:3][CH2:4][C:5]([O-:7])=[O:6].[Na+:22]

参加物

5

実験手順

A solution of t-butyl 4-hydroxy-4-(2-methylphenyl)butanoate, thought to be the (R)-enantiomer, (0.5 g) in tetrahydrofuran (3 mL) and methanol (3 mL) is treated with aqueous sodium hydroxide solution (5 N; 0.5 mL) and stirred at ambient temperature for 8 hours. The reaction mixture is concentrated to dryness. The resulting residue is treated with isopropanol (10 mL) and stirred for 30 minutes, and the resulting precipitate is collected and washed with isopropyl ether, to give sodium 4-hydroxy-4-(2-methylphenyl)butanoate, thought to be the (R)-enantiomer, (300 mg) in the form of a white solid, m.p. above 250° C.; 25[α]D=+34° (c=0.01; CH3OH); [NMR(DMSO-d6) (300 MHz):- 1.58-1.75 (m,2H),2.11(m,2H),2.22(s,3H),4.75(m,1H),7.05-7.48 (m.4H).

後処理

  1. concentrationThe reaction mixture is concentrated to dryness
  2. additionThe resulting residue is treated with isopropanol (10 mL)
  3. stirringstirred for 30 minutes
  4. customthe resulting precipitate is collected
  5. washwashed with isopropyl ether

出典と根拠

ORDレコード
ord-ced9dd7567274885b3435da95ecb6232
出典データセット
uspto-grants-2001_04
特許番号
US06211234B1

関連ノート

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