Oxalyl chloride → HCID 86666173、化合物

HRID 2405479

反応式

HRID 2405479 の反応式
[CH:1]([C@H:4]1[C@@H:8]2[C@@H:9]3[C@@:22]([CH3:25])([CH2:23][CH2:24][C@@:7]2([C:40]([OH:42])=O)[CH2:6][CH2:5]1)[C@@:21]1([CH3:26])[C@@H:12]([C@:13]2([CH3:39])[C@@H:18]([CH2:19][CH2:20]1)[C:17]([CH3:28])([CH3:27])[C@@H:16]([C:29]1[CH:34]=[CH:33][C:32]([C:35]([O:37][CH3:38])=[O:36])=[CH:31][CH:30]=1)[CH2:15][CH2:14]2)[CH2:11][CH2:10]3)([CH3:3])[CH3:2].C(Cl)(=O)C([Cl:46])=O>>[Cl:46][C:40]([C@:7]12[CH2:6][CH2:5][C@@H:4]([CH:1]([CH3:3])[CH3:2])[C@@H:8]1[C@@H:9]1[C@@:22]([CH3:25])([CH2:23][CH2:24]2)[C@@:21]2([CH3:26])[C@@H:12]([C@:13]3([CH3:39])[C@@H:18]([CH2:19][CH2:20]2)[C:17]([CH3:27])([CH3:28])[C@@H:16]([C:29]2[CH:34]=[CH:33][C:32]([C:35]([O:37][CH3:38])=[O:36])=[CH:31][CH:30]=2)[CH2:15][CH2:14]3)[CH2:11][CH2:10]1)=[O:42]

参加物

3

実験手順

To a flask containing (1S,3aS,5aR,5bR,7aS,9S,11aS,11bR,13aR,13bR)-1-isopropyl-9-(4-(methoxycarbonyl)phenyl)-5a,5b,8,8,11a-pentamethylicosahydro-1H-cyclopenta[a]chrysene-3a-carboxylic acid (0.154 g, 0.267 mmol) was added oxalyl chloride (2M in dichloromethane) (5 mL, 10.00 mmol). The solution was stirred at rt for 3 h. The mixture was concentrated under reduced pressure and was dissolved in dichloromethane and concentrated two additional times. The crude product was used in the next step with no additional purification.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. dissolutionwas dissolved in dichloromethane
  3. concentrationconcentrated two additional times
  4. customThe crude product was used in the next step with no additional purification

出典と根拠

ORDレコード
ord-983612fc2bb74adca3ac9db488f87d53
出典データセット
uspto-grants-2014_08
特許番号
US08802661B2

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