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Hydrochloric Acid → 3-Acetoxy-5-biphenyl-4-yl-pentanoic acid tert-butyl ester

HRID 1297256
ノート
印刷プレビュー

反応式

HRID 1297256 の反応式
[C:1](OC(=O)C)(=[O:3])[CH3:2].[C:8]([O:12][C:13](=[O:31])[CH2:14][CH:15]([OH:30])[CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:20][CH:19]=1)([CH3:11])([CH3:10])[CH3:9].N1C=CC=CC=1.Cl>CN(C)C1C=CN=CC=1.ClCCl>[C:8]([O:12][C:13](=[O:31])[CH2:14][CH:15]([O:30][C:1](=[O:3])[CH3:2])[CH2:16][CH2:17][C:18]1[CH:19]=[CH:20][C:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:22][CH:23]=1)([CH3:11])([CH3:9])[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 116240165-Biphenyl-4-yl-3-hydroxy-pentanoic acid tert-butyl ester2 回

生成物 1

HCID 586751293-Acetoxy-5-biphenyl-4-yl-pentanoic acid tert-butyl ester収率 74%

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒2 回

実験手順

Acetic anhydride (40 μL, 0.42 mmol) was added to a stirred solution of 5-biphenyl-4-yl-3-hydroxy-pentanoic acid tert-butyl ester (Intermediate 3, 54 mg, 0.17 mmol), 4-dimethylaminopyridine (5.0 mg, 41 μmol) and pyridine (54 μL, 0.66 mol) in dichloromethane (1 mL) at room temperature under nitrogen. Stirring was continued for 12 hours at room temperature before the addition of 2 M hydrochloric acid (5 mL) and dichloromethane (5 mL). The phases were separated and aqueous phase extracted with dichloromethane (3×5 mL). The organic phases were combined, washed with brine (5 mL) and dried (MgSO4). The solvent was removed by evaporation under reduced pressure to give the title compound (45 mg, 74%) as a colourless gum. LC/MS: 3.91 min; z/e 386, calcd (M+NH4) 386. 1H NMR (400 MHz: CDCl3): 7.59 (2 H), 7.52 (2 H), 7.42 (2 H), 7.33 (1 H), 7.25 (2 H), 5.29 (1 H), 2.70 (2 H), 2.53 (2 H), 2.05 (3 H), 1.97 (2H), 1.42 (9 H).

後処理

  1. customThe phases were separated
  2. extractionaqueous phase extracted with dichloromethane (3×5 mL)
  3. washwashed with brine (5 mL)
  4. dry with materialdried (MgSO4)
  5. customThe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-62d54a42bcec4fe7a53ed57b89d42e65
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07250439B2

反応ノート

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