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HRID 629668作成日:2026年10月26日

Di-tert-butyl glutamate hydrochloride → di-tert-butyl N-(4-(tert-butoxycarbonylamino)-2-nitrobenzamido)-L-glutamate

https://huagongshe.com/reaction/629668

反応式

関与物質

役割名称HCID仕込み量
反応物Di-tert-butyl glutamate hydrochlorideHCID 208636—
反応物Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 2733084—
反応物4-{[(Tert-butoxy)carbonyl]amino}-2-nitrobenzoic acidHCID 21951876—
溶媒DichloromethaneHCID 6344—
溶媒TriethylamineHCID 8471—
生成物di-tert-butyl N-(4-(tert-butoxycarbonylamino)-2-nitrobenzamido)-L-glutamateHCID 68695638—

反応手順

To a mixture of 4-(tert-butoxycarbonylamino)-2-nitrobenzoic acid in 60 ml of dichloromethane were added 4.8 g of N,N,N′,N′-tetramethyl-O-(1H-benzotriazol-1-yl)-uronium-hexafluorophosphate. After stirring for 15 min. a mixture of 3.8 g of L-glutamic acid-di tert.-butylester hydrochloride in 60 ml dichloromethane and 3 ml triethylamine was added dropwise. After stirring for 20 hours at room temperature, the mixture was filtered and the filtrate was washed five times with 10% aqueous citric acid, four times with 5% aqueous sodium carbonate solution and two times with water. The organic layer was dried over magnesium sulphate and concentrated in vacuum to give 6.3 g of di-tert-butyl N-(4-(tert-butoxycarbonylamino)-2-nitrobenzamido)-L-glutamate as a yellow foam. This was directly used in example 3.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09315506B2
出典データセットuspto-grants-2016_04
ORD IDord-5050c73064234dc0801cc0c6f60729b4
出典メモuspto-grants-2016_04