Conessine → HCID 67424844, 화합물

HRID 1393021노트

반응식

HRID 1393021 반응식
[CH3:1][C@@H:2]1[N:25]([CH3:26])[CH2:24][C@:7]23[CH2:8][CH2:9][C@@H:10]4[C@@:15]5([CH3:23])[CH2:16][CH2:17][C@H:18]([N:20]([CH3:22])[CH3:21])[CH2:19][C:14]5=[CH:13][CH2:12][C@H:11]4[C@@H:6]2[CH2:5][CH2:4][C@H:3]13>C(OCC)(=O)C.[Pd]>[CH3:21][N:20]([CH3:22])[CH:18]1[CH2:19][CH:14]2[C:15]([CH3:23])([CH:10]3[CH:11]([CH2:12][CH2:13]2)[CH:6]2[CH2:5][CH2:4][CH:3]4[CH:2]([CH3:1])[N:25]([CH3:26])[CH2:24][C:7]24[CH2:8][CH2:9]3)[CH2:16][CH2:17]1

참가 물질

4

반응물 1

HCID 441082Conessine

생성물 1

HCID 67424844HCID 67424844, 화합물수율 30%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

Conessine (50 mg, 0.14 mmol) was dissolved in 3 mL ethyl acetate and 10% Pd/C (20 mg) was added under inert atmosphere. The reaction mixture was hydrogenated under a hydrogen balloon for 24 hours. Reaction was not complete by TLC. The reaction mixture was filtered through diatomaceous earth, washed with ethyl acetate, and the filtrate was concentrated to give the crude product which was purified by silica gel column eluted with 0.3% ammonium hydroxide and 3% methanol in dichloromethane to give the desired product (15 mg, 30% yield).

후처리

  1. customfor 24 hours
  2. customReaction
  3. filtrationThe reaction mixture was filtered through diatomaceous earth
  4. washwashed with ethyl acetate
  5. concentrationthe filtrate was concentrated
  6. customto give the crude product which
  7. customwas purified by silica gel column
  8. washeluted with 0.3% ammonium hydroxide and 3% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-7d80e4dff4eb410385c6a5258e7d98c8
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07345034B2

반응 노트

불러오는 중…