반응식
[CH2:1]([O:3][C:4](=[O:14])[CH:5]([NH:11][CH:12]=[O:13])/[CH:6]=[C:7](\[CH3:10])/[CH2:8]Br)[CH3:2].[Cl:15][CH2:16][CH2:17][O:18][P:19]([O:24]CCCl)[O:20][CH2:21][CH2:22][Cl:23]>>[CH2:1]([O:3][C:4](=[O:14])[CH:5]([NH:11][CH:12]=[O:13])/[CH:6]=[C:7](\[CH3:10])/[CH2:8][P:19]([O:20][CH2:21][CH2:22][Cl:23])([O:18][CH2:17][CH2:16][Cl:15])=[O:24])[CH3:2]참가 물질
3
실험 절차
8.2 g of E-5-bromo-2-formylamino-4-methyl-3-pentenoic acid ethyl ester and 19 ml of tris-(2-chloroethyl)-phosphite are stirred at a bath temperature of 70° for 20 hours. The resulting mixture is chromatographed on silica gel using ethyl acetate and ethyl acetate/isopropanol (7:1) as eluant, and the product is crystallised from ethyl acetate/diethyl ether. In this manner there is obtained E-2-formylamino-4-methyl-5-di(2-chloroethyl)phosphono-3-pentenoic acid ethyl ester, m.p. 47°-49°.
후처리
- customThe resulting mixture is chromatographed on silica gel
- customthe product is crystallised from ethyl acetate/diethyl ether
출처 및 근거
- ORD 기록
- ord-1a534022893b4efaaa29cf12b1d495e6
- 출처 데이터셋
- uspto-grants-1991_09
- 특허 번호
- US05051413
연결된 노트
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