Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 2-Methylpentane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 5-Methylthiophene-2-carboxylic acid | HCID 74713 | — |
| 반응물 | Propylphosphonic anhydride | HCID 111923 | — |
| 반응물 | Tert-butyl 1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate hydrochloride | HCID 66964240 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Methylpentane | HCID 7892 | — |
| 생성물 | Tert-butyl 4-(5-methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate | HCID 57989101 | — |
반응 단계
1-Propanephosphonic acid cyclic anhydride (1.57M solution in THF, 0.64 mL) was added to a solution of tert-butyl 1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate hydrochloride (WuXi PharmaTech) (0.26 g), 5-methylthiophene-2-carboxylic acid (0.142 g) and triethylamine (0.84 mL) in DMF (8 mL) and the resulting mixture stirred for 16 h. The reaction mixture was poured into water (100 mL) and extracted with ethyl acetate (3×200 mL). The combined organic solutions were washed with water (2×100 mL) and brine (100 mL), then dried over magnesium sulphate, filtered and evaporated in vacuo. Purification was by silica gel chromatography eluting with ethyl acetate:isohexane, 1:1 to give the subtitled compound as a clear oil. Yield 0.32 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08148373B2 |
| 출처 데이터셋 | uspto-grants-2012_04 |
| ORD ID | ord-2bea720a39d74bf59b258f8b62f8270c |
| 출처 메모 | uspto-grants-2012_04 |