Methanol → Methyl 11-bromoundecanoate

HRID 653348

반응식

HRID 653348 반응식
[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]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1781211-Bromoundecanoic acidHCID 5284359Calcium Chloride

생성물 1

HCID 223913Methyl 11-bromoundecanoate수율 84%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-602b2bdb47f54c15b743da6bba95f29f
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675392

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