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Sodium hydride → HCID 86760615、化合物

HRID 2057045
ノート
印刷プレビュー

反応式

HRID 2057045 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:10])[C@H:6]([CH3:9])[NH:7][CH3:8])[CH3:3].[H-].[Na+].[C:13]([S:16][CH2:17][CH2:18][C:19](Cl)=[O:20])(=[O:15])[CH3:14].C(=O)(O)[O-].[Na+]>O1CCCC1>[CH2:2]([O:4][C:5](=[O:10])[C@@H:6]([N:7]([C:19](=[O:20])[CH2:18][CH2:17][S:16][C:13](=[O:15])[CH3:14])[CH3:8])[CH3:9])[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 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 129431223-(Acetylsulfanyl)propanoyl chlorideHCID 86621252(S)-2-methylaminopropionic acid ethyl esterhydrochloride

生成物 1

HCID 86760615HCID 86760615、化合物収率 75.2%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

The solution of 15 g (89.5 mmol) of N-methylalanine ethyl ester-hydrochloride in 850 ml of anhydrous tetrahydrofuran is mixed at 23° C. with 4.1 g of an approximately 60% sodium hydride dispersion and, after 3 hours, with 23.5 g of 3-acetylsulfanyl-propanoic acid chloride. It is allowed to react for two days, mixed with saturated sodium bicarbonate solution, and extracted several times with ethyl acetate. The combined organic extracts are washed with saturated sodium chloride solution, dried over sodium sulfate, and the residue that is obtained after filtration and removal of the solvent is purified by chromatography on fine silica gel. 17.6 g (67.3 mmol, 75%) of the title compound is isolated as a colorless oil.

後処理

  1. customto react for two days
  2. extractionextracted several times with ethyl acetate
  3. washThe combined organic extracts are washed with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customthe residue that is obtained
  6. filtrationafter filtration and removal of the solvent
  7. customis purified by chromatography on fine silica gel

出典と根拠

ORDレコード
ord-27a0a73ea9004911afff0eb8fa500f3c
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07335775B2

反応ノート

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