Carbon tetrabromide → tert-Butyl 3-bromopropionate
반응식
[C:1]([O:5][C:6](=[O:10])[CH2:7][CH2:8]O)([CH3:4])([CH3:3])[CH3:2].C(Br)(Br)(Br)[Br:12].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(#N)C>[C:1]([O:5][C:6](=[O:10])[CH2:7][CH2:8][Br:12])([CH3:4])([CH3:3])[CH3:2]참가 물질
5
실험 절차
3-Hydroxy-propionic acid tert-butyl ester is dissolved in acetonitrile and carbon tetrabromide and triphenylphosphine is added. The mixture is stirred at room temperature overnight. After this time the mixture is concentrated in vacuo. The gummy solid is triturated with hexanes and the liquid decanted, passed through pad of silica to remove any triphenylphosphine oxide, and concentrated in vacuo. 1H NMR (400 MHz, CHLOROFORM-d) ppm 1.3 (9H, s), 2.06-2.27 (2H, m), 4.07-4.25 (2H, m).
후처리
- concentrationAfter this time the mixture is concentrated in vacuo
- customThe gummy solid is triturated with hexanes
- customthe liquid decanted
- customto remove any triphenylphosphine oxide
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-dcb257f0551e46a2852671ecd9f8e2c7
- 출처 데이터셋
- uspto-grants-2014_01
- 특허 번호
- US08629157B2
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