Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 11-[2,3-Difluorobiphenyl-4'-yl]oxyundecyl 2,2-bis(6-benzyloxyhexyl)acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 반응물 | HCID 18920839 | HCID 18920839 | — |
| 반응물 | 2,3-Difluoro-4'-(11-hydroxyundecyl)oxybiphenyl | HCID 18920844 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 11-[2,3-Difluorobiphenyl-4'-yl]oxyundecyl 2,2-bis(6-benzyloxyhexyl)acetate | HCID 18920866 | 92.6% |
반응 단계
First, 3.0 g of 2,2-bis(6-benzyloxyhexyl)acetic acid, 2.8 g of 2,3-difluoro-4'-[11-hydroxyundecyl]oxybiphenyl, 2.2 g of triphenylphosphine, and 50 ml of tetrahydrofuran were placed in a 100 ml flask. Then, 1.4 g of diethyl azodicarboxylate was added dropwise to the mixture at 5° C. The resultant mixture was allowed to warm to room temperature and stirred for 8 hours. The reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/9) to obtain 5 g of 11-[2,3-difluorobiphenyl-4'-yl]oxyundecyl 2,2-bis(6-benzyloxyhexyl)acetate (Y: 92.6%). The compound thus obtained had a purity of 98% by HPLC.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05750213 |
| 출처 데이터셋 | uspto-grants-1998_05 |
| ORD ID | ord-629fdf332b6940b7804f2ddc3ea63451 |
| 출처 메모 | uspto-grants-1998_05 |