Water → Hexamethyldisiloxane

HRID 1706040

反応式

HRID 1706040 の反応式
[CH3:1][C@@H:2]([C@@H:10]1[C@@:14]2([CH3:29])[CH2:15][CH2:16][CH2:17]/[C:18](=[CH:19]\[CH:20]=[C:21]3\[CH2:22][C@@H:23]([OH:28])[CH2:24][CH2:25][C:26]\3=[CH2:27])/[C@@H:13]2[CH2:12][CH2:11]1)[CH2:3][CH2:4][CH2:5][C:6]([OH:9])([CH3:8])[CH3:7].C(Cl)(=O)C1C=CC=CC=1.[CH3:39][Si:40]([CH3:43])([CH3:42])Cl.[OH2:44]>N1C=CC=CC=1.CN(C1C=CN=CC=1)C>[CH3:1][C@@H:2]([C@@H:10]1[C@@:14]2([CH3:29])[CH2:15][CH2:16][CH2:17]/[C:18](=[CH:19]\[CH:20]=[C:21]3\[CH2:22][C@@H:23]([OH:28])[CH2:24][CH2:25][C:26]\3=[CH2:27])/[C@@H:13]2[CH2:12][CH2:11]1)[CH2:3][CH2:4][CH2:5][C:6]([OH:9])([CH3:7])[CH3:8].[CH3:39][Si:40]([O:44][Si:40]([CH3:43])([CH3:42])[CH3:39])([CH3:43])[CH3:42]

参加物

8

反応物 4

HCID 962WaterHCID 6397ChlorotrimethylsilaneHCID 7412Benzoyl chlorideHCID 528373125-Hydroxyvitamin D3

生成物 2

HCID 24764HexamethyldisiloxaneHCID 528373125-Hydroxyvitamin D3

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

To a solution of 25-hydroxycholecalciferol (5.0 g.) in pyridine (25 ml.) at -15°, under an atmosphere of argon, is added 4-(N,N-dimethylamino)-pyridine (50 mg) followed by benzoyl chloride (2.10 ml.). The solution is warmed to 0° and kept at this temperature for 1.5 hours. After cooling to -15°, trimethylchlorosilane (1.75 ml.) is added and then the mixture is heated to room temperature for 10 minutes, before pouring into water. The mixture is extracted with hexane (500 ml.) and the extracts washed with brine, dilute hydrochloric acid, brine, sodium bicarbonate solution, brine and then dried over sodium sulfate. Evaporation of the solution yields 25-hydroxycholecalciferol, 3-benzoate, trimethylsilylether as an oil.

後処理

  1. temperatureThe solution is warmed to 0°
  2. temperatureAfter cooling to -15°
  3. extractionThe mixture is extracted with hexane (500 ml.)
  4. washthe extracts washed with brine, dilute hydrochloric acid, brine, sodium bicarbonate solution, brine
  5. dry with materialdried over sodium sulfate
  6. customEvaporation of the solution

出典と根拠

ORDレコード
ord-bd3e980da6fa4280906293410f0432c2
出典データセット
uspto-grants-1980_06
特許番号
US04206131

関連ノート

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