Conessine → HCID 67424844、化合物

HRID 1393021ノート

反応式

HRID 1393021 の反応式
[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

参加物

4

反応物 1

HCID 441082Conessine

生成物 1

HCID 67424844HCID 67424844、化合物収率 30%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7d80e4dff4eb410385c6a5258e7d98c8
出典データセット
uspto-grants-2008_03
特許番号
US07345034B2

反応ノート

読み込み中…