Tributylamine → Cholesterol

HRID 441432

反応式

HRID 441432 の反応式
[CH3:1][C@@H:2]([C@@H:9]1[C@@:13]2([CH3:35])[CH2:14][CH2:15][C@@H:16]3[C@@:21]4([CH3:34])[CH2:22][CH2:23][C@H:24]([O:26]C(CCC(O)=O)=O)[CH2:25][C:20]4=[CH:19][CH2:18][C@H:17]3[C@@H:12]2[CH2:11][CH2:10]1)[CH2:3][CH2:4][CH2:5][CH:6]([CH3:8])[CH3:7].C(N(CCCC)CCCC)CCC.ClC(OCC(C)C)=O.[OH-].[Na+]>O1CCOCC1.O>[CH3:8][CH:6]([CH2:5][CH2:4][CH2:3][C@H:2]([C@@H:9]1[C@:13]2([CH3:35])[C@H:12]([C@H:17]3[C@H:16]([CH2:15][CH2:14]2)[C@:21]2([CH3:34])[C:20]([CH2:25][C@H:24]([CH2:23][CH2:22]2)[OH:26])=[CH:19][CH2:18]3)[CH2:11][CH2:10]1)[CH3:1])[CH3:7]

参加物

7

反応物 4

HCID 7622TributylamineHCID 14798Sodium HydroxideHCID 62365Isobutyl chloroformateHCID 65082Cholesteryl hemisuccinate

生成物 1

HCID 5997Cholesterol

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

20.25 Grams (41.8 mmoles) of cholesteryl hydrogen succinate (sold by Aldrich Chemicals) and 19.8 ml (83.4 mmoles) of tributylamine were dissolved in 540 ml of Dioxane. The solution was cooled and treated with 5.3 ml (5.7 g, 41.7 mmoles) of isobutyl chloroformate. The reaction was permitted to proceed in the cold for 30 minutes, and then the mixture was added in one portion to a stirred, cooled solution of 50.0 g (41.7 moles) of bovine serum albumin in 1100 ml of water, 750 ml of p-dioxane, and 50 ml of 1 N NaOH. Stirring and cooling was continued for 6 hours. The material was then dialyzed against water and lyophilized to yield a stable white powder useful as a cholesterol standard.

後処理

  1. temperatureThe solution was cooled
  2. customcold for 30 minutes
  3. additionthe mixture was added in one portion to a stirred
  4. temperaturecooling
  5. customThe material was then dialyzed against water

出典と根拠

ORDレコード
ord-4205418b42e845479236a25c00939090
出典データセット
uspto-grants-1977_08
特許番号
US04040784

関連ノート

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