Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Methylmorpholine → 2-Hydroxy-2,4-dimethyl-3-pentanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | Ethyl chloroformate | HCID 10928 | — |
| 반응물 | 3-Amino-2,4-dimethylpentan-2-ol | HCID 13247948 | — |
| 반응물 | N-benzyloxycarbonyl-beta-benzyl-L-aspartyl-D-alanine | HCID 53966575 | — |
| 촉매 | Dihydroxy(dioxo)molybdenum;phosphonic acid | HCID 21863154 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl acetate hexane | HCID 21226206 | — |
| 생성물 | 2-Hydroxy-2,4-dimethyl-3-pentanone | HCID 547735 | — |
반응 단계
To a solution of 2.14 g. (5.0 mmole) beta-benzyl-N-benzyloxycarbonyl-L-aspartyl-D-alanine in 35 ml. tetrahydrofuran cooled to -15° was added 0.55 ml. (5.0 mmole) N-methylmorpholine and 0.48 ml. (5.0 mmole) ethyl chloroformate. The mixture was stirred at -15° to -10° C. for two minutes and 0.66 g. (5.0 mmole) 3-amino-2-hydroxy-2,4-dimethylpentane was added. The mixture was allowed to warm to room temperature, stirred overnight and worked-up as described in Example 5, Part B, to obtain the diprotected dipeptide amide, Rf 0.27 (TLC, ethyl acetate/hexane, 1:1, phosphomolybdic acid spray, heat) which was used directly in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04894464 |
| 출처 데이터셋 | uspto-grants-1990_01 |
| ORD ID | ord-079a054ae14c446cae2a98d5a52d1fe9 |
| 출처 메모 | uspto-grants-1990_01 |