반응 #220447

ord-daefbfbb18364f409a9946b7f6f61661

반응 조건

온도
-23°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was prepared as a white solid
  2. 2
    기타Purification
  3. 3
    세척eluting with CH2Cl2/MeOH (98:2 gradient to 95:5
  4. 4
    기타with 5% NH3 in the MeOH) followed by recrystallization

실험 절차

Following General Procedure 8-L using the product from Step B, 3-amino-2,4-dioxo-1,5-bis-cyclopropylmethyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine was prepared as a white solid. Purification was by flash chromatography eluting with CH2Cl2/MeOH (98:2 gradient to 95:5, with 5% NH3 in the MeOH) followed by recrystallization from warm CH2Cl2/hexanes (1:1) to −23° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07390801B2uspto-grants-2008_06