참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Chloroethyl formate | HCID 246748 | — |
| 반응물 | 1-Benzhydryl-3-[5-bromo-2-(3-chloro-benzyloxy)-phenoxy]-3-methyl-azetidine | HCID 67348353 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 3-[5-Bromo-2-(3-chloro-benzyloxy)-phenoxy]-3-methyl-azetidine | HCID 46214971 | 71.7% |
반응 단계
The title compound from Step B (60 mg) was dissolved in DCE (10 mL) and chloroethylformate (0.2 mmol) was added. The mixture was heated at 80-100° C. for 1 h and concentrated. The residue was dissolved in MeOH (3 mL) and heated at 150° C. in a microwave reactor for another 1 h. The mixture was cooled to rt and purified via PTLC providing the title compound (30 mg). MS (ESI): mass calcd. for C17H17BrClNO2, 381.0; m/z found, 382.0 [M+H]+. 1H NMR (CDCl3): 7.43-7.23 (m, 4H), 7.12-7.06 (m, 1H), 6.86-6.78 (m, 2H), 5.12 (s, 2H), 4.24-4.16 (m, 2H), 3.78-3.67 (m, 2H), 1.67 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08642583B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-dd072f025a254296a3caa4036aa28404 |
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| 출처 메모 | uspto-grants-2014_02 |
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