반응 #159352

ord-66d0a3bbbf7847b5886cbbd27d02ae96

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The crude product was purified by gradient flash chromatography (methanol/methylene chloride) on a RediSep disposable column

실험 절차

The resulting product from Step 1 was deprotected in a similar manner as Example 1, step 3, and the compound was used immediately and coupled to N-Cbz-L-valine in accordance with the procedures set forth in Example 12, Method B. The crude product was purified by gradient flash chromatography (methanol/methylene chloride) on a RediSep disposable column. 1H NMR (CD3Cl, 300 MHz): δ 7.45-7.25 (m, 10H), 6.0-5.85 (m, 1H), 5.18-4.92 (m, 4H), 4.50-4.33 (m, 2H), 4.31-4.04 (m, 2H), 3.43-3.26 (m, 2H), 2.25-2.03 (m, 3H), 2.02-1.70 (m, 8H), 1.37-1.10 (m, 4H), 1.04-0.82 (m, 20H). LCMS m/z: [M+H]+=757.9.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08828974B2uspto-grants-2014_09