N-bromobutanimide → HCID 86718010, 화합물

HRID 1500472노트

반응식

HRID 1500472 반응식
[CH3:1][C@@H:2]1[CH2:6][C:5]2[CH:7]=[C:8]([CH3:12])[CH:9]=[C:10]([NH2:11])[C:4]=2[O:3]1.C1C(=O)N([Br:20])C(=O)C1>CN(C=O)C>[Br:20][C:7]1[C:5]2[CH2:6][C@@H:2]([CH3:1])[O:3][C:4]=2[C:10]([NH2:11])=[CH:9][C:8]=1[CH3:12]

참가 물질

4

반응 조건

온도
0 °C

실험 절차

To a mixture of (R)-2,5-dimethyl-2,3-dihydrobenzofuran-7-amine (3f) (1.3 g, 7.9 mmol) in DMF (16 mL) was added NBS (1.42 g, 7.9 mmol) at 0° C. It was stirred for 15 min at 0° C. The mixture was extracted with EtOAc (150 mL), washed with NaHSO3 (50 mL), water and brine, dried and concentrated. The residue was purified by column chromatography on silica gel eluting with hexanes/EtOAc (20:1) to give the title compound (3g) as a solid. MS-ESI (m/z): 242 (M+1)+.

후처리

  1. extractionThe mixture was extracted with EtOAc (150 mL)
  2. washwashed with NaHSO3 (50 mL), water and brine
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on silica gel eluting with hexanes/EtOAc (20:1)

출처 및 근거

ORD 기록
ord-d3f31bc6cd614a608d23b655ff0fbfc2
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206166B2

반응 노트

불러오는 중…