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Cholesterol → 25279-63-4

HRID 511732
ノート
印刷プレビュー

反応式

HRID 511732 の反応式
[CH3:1][CH:2]([CH2:4][CH2:5][CH2:6][C@H:7]([C@@H:9]1[C@:27]2([CH3:28])[C@H:12]([C@H:13]3[C@H:24]([CH2:25][CH2:26]2)[C@:22]2([CH3:23])[C:16]([CH2:17][C@H:18]([CH2:20][CH2:21]2)[OH:19])=[CH:15][CH2:14]3)[CH2:11][CH2:10]1)[CH3:8])[CH3:3].C(N(CC)CC)C.[N+:36]([C:39]1[CH:40]=[C:41]([CH:45]=[C:46]([N+:48]([O-:50])=[O:49])[CH:47]=1)[C:42](Cl)=[O:43])([O-:38])=[O:37]>CN(C)C1C=CN=CC=1.ClCCl>[N+:36]([C:39]1[CH:40]=[C:41]([CH:45]=[C:46]([N+:48]([O-:50])=[O:49])[CH:47]=1)[C:42]([O:19][C@H:18]1[CH2:20][CH2:21][C@@:22]2([CH3:23])[C:16](=[CH:15][CH2:14][C@@H:13]3[C@@H:24]2[CH2:25][CH2:26][C@@:27]2([CH3:28])[C@H:12]3[CH2:11][CH2:10][C@@H:9]2[C@H:7]([CH3:8])[CH2:6][CH2:5][CH2:4][CH:2]([CH3:1])[CH3:3])[CH2:17]1)=[O:43])([O-:38])=[O:37]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 5997CholesterolHCID 74323,5-Dinitrobenzoyl chlorideHCID 8471Triethylamine

生成物 1

HCID 2111671025279-63-4収率 56.4%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344
Dichloromethane
溶媒
2 回

反応条件

温度
0 °C

実験手順

20.00 g (51.7 mmol) of cholesterol, 2.88 g (25.75 mmol) of 4-dimethylaminopyridine, 6.27 g (62.04 mmol) of triethylamine are dissolved in 100 mL of dichloromethane. 11.92 g (51.7 mmol) of commercial 3,5-dinitrobenzoylchloride dissolved in 50 mL of dichloromethane are added at 0° C. The solution is stirred for 2 h at 0° C. and allowed to stir at room temperature overnight. After 22 hours at room temperature, the reaction mixture is partitioned between dichloromethane and water. The organic phase is washed repeatedly with water, dried over sodium sulfate, filtrated and concentrated under reduced pressure. Crystallization from ethyl acetate:hexane mixture yielded 16.94 g (56%) of (3-β)-cholest-5-en-3-yl 3,5-dinitrobenzoate as yellowish crystals.

後処理

  1. additionare added at 0° C
  2. stirringto stir at room temperature overnight
  3. waitAfter 22 hours at room temperature
  4. customthe reaction mixture is partitioned between dichloromethane and water
  5. washThe organic phase is washed repeatedly with water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltrated
  8. concentrationconcentrated under reduced pressure
  9. customCrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-aebcc1a4cc8b4ab3a53d9eb5b82a5040
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09097938B2

反応ノート

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