참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Benzoyl chloride | HCID 7412 | — |
| 반응물 | Methyl N-(diphenylmethylidene)glycinate | HCID 563248 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Amino-3-oxo-3-phenylpropionic acid methylester | HCID 13290648 | 80.9% |
반응 단계
Dry tetrahydrofuran (250 ml) was cooled to -78° C. Potassium tert-butoxide (6.37 g; 56.72 mmol) was dissolved in dry tetrahydrofuran (100 ml) and added. (Benzhydrylideneamino)acetic acid methyl ester (14.35 g; 56.72 mmol) was added and the reaction mixture was stirred 30 min at -78° C. Benzoyl chloride (6.59 g; 56.72 mmol) was added dropwise and the reaction mixture was stirred 30 min at -78° C. Hydrochloric acid (1.0 M; 175 ml) was added dropwise. The reaction mixture was heated to room temperature and 2/3 of the solvent was removed in vacuo. Water (700 ml) was added and the reaction mixture was washed with diethyl ether (400 ml). The aqueous phase was evaporated in vacuo and the residue was dissolved in methanol and evaporated (2×150 ml). Methanol (80 ml) was added. The mixture was filtrated and the filtrate was evaporated in vacuo. The residue was recrystallised from tetrahydrofuran/diethyl ether to afford 8.86 g of 2-amino-3-oxo-3-phenylpropionic acid methylester as a hydrochloride.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06013658 |
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| 출처 데이터셋 | uspto-grants-2000_01 |
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| ORD ID | ord-1a33de8d65b34484873978489d505875 |
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| 출처 메모 | uspto-grants-2000_01 |
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