Phenylethanolamine → HCID 57495437、化合物

HRID 1039152ノート

反応式

HRID 1039152 の反応式
[NH2:1][CH2:2][CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[CH3:11][O:12][C:13](=[O:23])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20](O)=[O:21].ON1C2C=CC=CC=2N=N1>C1COCC1.C(OCC)(=O)C>[CH3:11][O:12][C:13](=[O:23])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20](=[O:21])[NH:1][CH2:2][CH:3]([OH:4])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

6

反応物 3

HCID 1000PhenylethanolamineHCID 757711-HydroxybenzotriazoleHCID 5541918-Methoxy-8-oxooctanoic acid

生成物 1

HCID 57495437HCID 57495437、化合物収率 92.1%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Add 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide(EDC) (8.5 g, 44.3 mL) to a solution of 2-amino-1-phenylethanol (5.0 g, 36.4 mmol), suberic acid monomethyl ester (6.85 g, 36.4 mmol) and 1-hydroxybenzotriazole (HOBt, 5.0 g, 37.0 mmol) in THF (200 mL) at room temperature under nitrogen. Stir the mixture for 12 hours. Dilute the mixture with ethyl acetate (600 mL), wash with 1N HCl (2×150 mL), brine (2×150 mL), NaHCO3 (2×150 mL) and brine (150 mL) solutions and dry over sodium sulfate. Remove the solvent under reduced pressure to provide 7-(2-hydroxy-2-phenylethylcarbamoyl)heptanoic acid methyl ester (10.3 g, 91%), which is used in the following step without purification.

後処理

  1. washwash with 1N HCl (2×150 mL), brine (2×150 mL), NaHCO3 (2×150 mL) and brine (150 mL) solutions
  2. dry with materialdry over sodium sulfate
  3. customRemove the solvent under reduced pressure

出典と根拠

ORDレコード
ord-8041fb1d28a240a39846c15891d0bf10
出典データセット
uspto-grants-2013_10
特許番号
US08552039B2

反応ノート

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