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Oxalyl chloride → (4-Bromomethyl-2-phenylbenzoyl)methionine methyl ester

HRID 2121203
ノート
印刷プレビュー

反応式

HRID 2121203 の反応式
[Br:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=O)=[C:5]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:4]=1.C(Cl)(=O)C(Cl)=O.Cl.[CH3:25][O:26][C:27](=[O:34])[C@H:28]([CH2:30][CH2:31][S:32][CH3:33])[NH2:29].C(N(C(C)C)CC)(C)C>ClCCl.CCOCC>[CH3:25][O:26][C:27](=[O:34])[C@H:28]([CH2:30][CH2:31][S:32][CH3:33])[NH:29][C:7](=[O:9])[C:6]1[CH:10]=[CH:11][C:3]([CH2:2][Br:1])=[CH:4][C:5]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
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 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 11435579L-Methionine, methyl ester, hydrochlorideHCID 234364554-Bromomethyl-2-phenylbenzoic acid

生成物 1

HCID 54323738(4-Bromomethyl-2-phenylbenzoyl)methionine methyl ester収率 75%

試薬・触媒・溶媒 2

HCID 3283
Diethyl Ether
溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution in dichloromethane (25 mL) of 4-bromomethyl-2-phenylbenzoic acid (2.16 g, 7.42 mmol), prepared as in Example 234B, was added oxalyl chloride (0.84 mL, 965 mmol) and 2 drops on DMF and the reaction mixture was stirred for 2 hours. The reaction mixture was concentrated in vacuo and azeotroped with toluene. The residue was dissolved in dichloromethane (15 mL) and then was added to a solution in dichloromethane (15 mL) of methionine methyl ester hydrochloride (1.78 g, 8.90 mmol) and diisopropylethylamine (3.10 g, 17.81 mmol) (prepared at −10° C.) dropwise. The reaction mixture was stirred for 30 minutes and then was poured into ether and extracted with water, aqueous 3N HCl (2×) and brine, dried, filtered and concentrated in vacuo. Chromatography on silica gel (5% ethyl acetate-chloroforn) to give (4-bromomethyl-2-phenylbenzoyl)methionine methyl ester (2.42 g, 75%).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customazeotroped with toluene
  3. dissolutionThe residue was dissolved in dichloromethane (15 mL)
  4. stirringThe reaction mixture was stirred for 30 minutes
  5. extractionextracted with water, aqueous 3N HCl (2×) and brine
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6535fdc3bacd48aea04de25869f6359c
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693123B2

反応ノート

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