참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | 1,2-Dibromoethane | HCID 7839 | — |
| 반응물 | Neophyl chloride | HCID 68191 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | beta-Phenylisovaleric acid | HCID 13890 | 81% |
반응 단계
Following a literature procedure, (Leffler, J. E.; Barbas, J. T. JACS. 1981, 103(26), 7768-7773), to a mixture of magnesium turnings (9.5 g) and neophyl chloride (7.5 mL) in tetrahydrofuran (100 mL) is added a spatula tip of iodine and 1,2-dibromoethane (1 mL). The mixture is heated gently with under a heat gun to initiate a vigorous reaction. A solution of neophyl chloride (57 mL) in tetrahydrofuran (360 mL) is added dropwise over the course of 90 minutes. Following completion of the addition, the reaction mixture is stirred for an additional five hours, then solid carbon dioxide (25 g) is added to the flask. After 10 minutes, the flask is transferred to a 40° C. water bath until all carbon dioxide had sublimed. The solvent is then removed under reduced pressure to afford the title compound (58 g, 81%) as a white paste. MS (ES+): (M+H)=178.8
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07390910B2 |
|---|
| 출처 데이터셋 | uspto-grants-2008_06 |
|---|
| ORD ID | ord-83009e25d2724ee08cd2ee2fd96be188 |
|---|
| 출처 메모 | uspto-grants-2008_06 |
|---|