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Triethylamine → HCID 178462020、化合物

HRID 1806724
ノート
印刷プレビュー

反応式

HRID 1806724 の反応式
Cl.[C:2]([O:6][C:7](=[O:11])[C@H:8]([CH3:10])[NH2:9])([CH3:5])([CH3:4])[CH3:3].[O-]S([O-])(=O)=O.[Mg+2].C(N(CC)CC)C.[CH3:25][C:26]([CH3:31])([CH3:30])[CH2:27][CH:28]=O>C(Cl)Cl>[C:2]([O:6][C:7](=[O:11])[C@@H:8](/[N:9]=[CH:28]/[CH2:27][C:26]([CH3:31])([CH3:30])[CH3:25])[CH3:10])([CH3:5])([CH3:4])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 763353,3-DimethylbutanalHCID 11275390tert-Butyl alaninate hydrochloride

生成物 1

HCID 178462020HCID 178462020、化合物収率 101.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

A mixture of L-alanine tert-butyl ester hydrochloride (Bachem) (1.8 g, 10 mmol) and MgSO4 in CH2Cl2 (100 mL) was added triethylamine (1.5 g, 15 mmol). The mixture was stirred at room temperature for 1 h, and 3,3-dimethyl-butyraldehyde (1 g, 10 mmol) was added. The reaction mixture was stirred at room temperature for 18 h. The mixture was filtered, and the filtrate was washed with water, brine, and concentrated. The residue was dried under reduced pressure to give (S)-2-[3,3-dimethyl-but-(E)-ylideneamino]-propionic acid tert-butyl ester as colorless oil (2.3 g, 100%) which was used without further purification.

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 18 h
  2. filtrationThe mixture was filtered
  3. washthe filtrate was washed with water, brine
  4. concentrationconcentrated
  5. customThe residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-f40bad915ad44f298c57993a44c13266
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354444B2

反応ノート

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