Methanol → Methyl 11-bromoundecanoate

HRID 653348

反応式

HRID 653348 の反応式
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13].[Cl-].[Ca+2].[Cl-].[CH3:18]O>>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH3:18])=[O:13]

参加物

4

反応物 3

HCID 887MethanolHCID 1781211-Bromoundecanoic acidHCID 5284359Calcium Chloride

生成物 1

HCID 223913Methyl 11-bromoundecanoate収率 84%

実験手順

11-Bromoundecanoic acid (commercial material, 25.0 g, 94 mmol), Duolite H+ resin (10 g), calcium chloride (26.2 g, 94 mmol) and methanol (700 ml) were stirred for 15 h. The methanol was removed and dichloromethane was added. The mixture was washed with water, dried (Na2SO4) and concentrated. Distillation gave pure 103 (22.0 g, 84%) with b.p. 103°-104° (2×10-2 torr). 1H-NMR (CDCl3, Me4Si) δ 3.67 (s, 3H, MeO), 3.41 (t, 2H, J=6.8 Hz, Br--CH2), 2.31 (t, 2H, J=7.3 Hz, CH2CO).

後処理

  1. customThe methanol was removed
  2. additiondichloromethane was added
  3. washThe mixture was washed with water
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated
  6. distillationDistillation

出典と根拠

ORDレコード
ord-602b2bdb47f54c15b743da6bba95f29f
出典データセット
uspto-grants-1987_06
特許番号
US04675392

関連ノート

読み込み中…