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Methanol → HCID 66558842、化合物

HRID 1530577
ノート
印刷プレビュー

反応式

HRID 1530577 の反応式
C(O[C:9]([N:11]1[CH2:16][CH2:15][CH:14]([CH:17]([O:22][C:23]2[CH:45]=[CH:44][C:26]3[C:27]4[N:31]([CH2:32][CH2:33][O:34][C:25]=3[CH:24]=2)[CH:30]=[C:29]([C:35]2[N:36]([CH:41]([CH3:43])[CH3:42])[N:37]=[C:38]([CH3:40])[N:39]=2)[N:28]=4)[C:18]([F:21])([F:20])[F:19])[CH2:13][CH2:12]1)=[O:10])C1C=CC=CC=1.CO.[CH3:48]CN(C(C)C)C(C)C.C(Cl)(=O)C>[Pd].CC(C)=O>[F:21][C:18]([F:19])([F:20])[CH:17]([CH:14]1[CH2:15][CH2:16][N:11]([C:9](=[O:10])[CH3:48])[CH2:12][CH2:13]1)[O:22][C:23]1[CH:45]=[CH:44][C:26]2[C:27]3[N:31]([CH:30]=[C:29]([C:35]4[N:36]([CH:41]([CH3:43])[CH3:42])[N:37]=[C:38]([CH3:40])[N:39]=4)[N:28]=3)[CH2:32][CH2:33][O:34][C:25]=2[CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 68313044HCID 68313044、化合物

生成物 1

HCID 66558842HCID 66558842、化合物収率 8.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 180
Acetone
溶媒

実験手順

To a solution of 4-{2,2,2-trifluoro-1-[2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-yloxy]ethyl}piperidine-1-carboxylic acid benzyl ester from Example 5 (210 mg, 0.34 mmol) in a 1:10 mixture MeOH:acetone (11 mL), was added 10% Pd/C (200 mg). The reaction mixture was stirred at RT under a hydrogen atmosphere for 18 h. The suspension was then filtered through a pad of Celite® and to the filtrate fresh 10% Pd/C (200 mg) was added. The reaction mixture was stirred at RT under a hydrogen atmosphere for 48 h. The suspension was then filtered through a pad of Celite® and the filtrate was concentrated in vacuo. The resulting residue was treated with DIPEA (0.79 mL, 4.42 mmol) and acetyl chloride (0.23 mL, 4.08 mmol) and stirred at RT for 18 h. The crude material was purified by reverse phase HPLC (Phenomenex Gemini 5 μm C18 on a 25 min gradient 10-90% 0.1% HCO2H in acetonitrile/water) affording 179 (15 mg, 8%). LCMS: RT 4.23 min [M+H]+ 533.2. 1H NMR (CDCl3, 400 MHz): δ 8.47 (1H, d, J=8.99 Hz), 7.61 (1H, s), 6.80 (1H, dd, J=9.00, 2.62 Hz), 6.64 (1H, d, J=2.49 Hz), 5.92-5.85 (1H, m), 4.78-4.69 (1H, m), 4.50-4.47 (2H, m), 4.46-4.35 (3H, m), 3.93-3.85 (1H, m), 3.16-3.02 (1H, m), 2.64-2.51 (1H, m), 2.42 (3H, s), 2.27-2.15 (1H, m), 2.10 (3H, d, J=2.36 Hz), 2.05-1.93 (1H, m), 1.89-1.75 (1H, m), 1.64-1.44 (8H, m)

後処理

  1. filtrationThe suspension was then filtered through a pad of Celite® and to the filtrate fresh 10% Pd/C (200 mg)
  2. additionwas added
  3. stirringThe reaction mixture was stirred at RT under a hydrogen atmosphere for 48 h
  4. filtrationThe suspension was then filtered through a pad of Celite®
  5. concentrationthe filtrate was concentrated in vacuo
  6. stirringstirred at RT for 18 h
  7. customThe crude material was purified by reverse phase HPLC (Phenomenex Gemini 5 μm C18 on a 25 min gradient 10-90% 0.1% HCO2H in acetonitrile/water)

出典と根拠

ORDレコード
ord-ac657198bf714cd3acbeab0c176f1b99
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090628B2

反応ノート

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