참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Di-tert-butyl glutamate hydrochloride | HCID 208636 | — |
| 반응물 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 반응물 | 4-{[(Tert-butoxy)carbonyl]amino}-2-nitrobenzoic acid | HCID 21951876 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | HCID 68695638 | HCID 68695638 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09315506B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-5050c73064234dc0801cc0c6f60729b4 |
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| 출처 메모 | uspto-grants-2016_04 |
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