(4-(Hydroxymethyl)phenyl)(phenyl)methanone → HCID 68506179、化合物

HRID 1881388ノート

反応式

HRID 1881388 の反応式
[CH2:1]([Sn:5]([CH2:12][CH2:13][CH2:14][CH3:15])([CH2:8][CH2:9][CH2:10][CH3:11])[O:6][CH3:7])[CH2:2][CH2:3][CH3:4].OC[C:18]1[CH:31]=[CH:30][C:21]([C:22]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:23])=[CH:20][CH:19]=1>ClCCCl>[CH2:8]([Sn:5]([CH2:1][CH2:2][CH2:3][CH3:4])([CH2:12][CH2:13][CH2:14][CH3:15])[O:6][CH2:7][C:27]1[CH:28]=[CH:29][C:24]([C:22]([C:21]2[CH:30]=[CH:31][CH:18]=[CH:19][CH:20]=2)=[O:23])=[CH:25][CH:26]=1)[CH2:9][CH2:10][CH3:11]

参加物

4

反応物 2

HCID 13149642(4-(Hydroxymethyl)phenyl)(phenyl)methanoneHCID 16683411Tributyltin methoxide

生成物 1

HCID 68506179HCID 68506179、化合物収率 56.2%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

In a 50 ml dry three-neck-flask, 2.5 g (7.8 mmol) of tri-n-butylmethoxy tin are added to 1.5 g (7.1 mmol) of 4-(hydroxymethyl)-benzophenone in 15 ml of 1,2-dichlorethane at room temperature in the course of 0.5 h under argon. 1H-NMR-spectrum confirms the complete conversion. The solution is concentrated and the crude product, 3.6 g of a yellow oil, is distilled in a bulb-to-bulb distillation apparatus in vacuum (0.016 mbar) at 160-170° C. The resulting colorless oil (2.8 g) is distilled a second time in a bulb-to-bulb distillation apparatus (0.020 mbar). 2.0 g of the title product are obtained as a colorless oil (boiling area 294-308° C.). The structure is further confirmed by 1H-NMR and 13C-NMR-spectra.

後処理

  1. customIn a 50 ml dry three-neck-flask
  2. concentrationThe solution is concentrated
  3. distillationthe crude product, 3.6 g of a yellow oil, is distilled in a bulb-to-bulb distillation apparatus in vacuum (0.016 mbar) at 160-170° C
  4. distillationThe resulting colorless oil (2.8 g) is distilled a second time
  5. distillationin a bulb-to-bulb distillation apparatus (0.020 mbar)

出典と根拠

ORDレコード
ord-15cee02d21e247cd9dd3c0f2916c717f
出典データセット
uspto-grants-2012_11
特許番号
US08318830B2

反応ノート

読み込み中…