반응 #1375813

ord-871560983abd480daa5fe2479ef7f7f5

반응 방정식

CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccc(C(=O)OC)cc1
methyl 4-tri-n-butylstannylbenzoate
[K+].[OH-]
KOH
CC(=O)O
acetic acid
O
water
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccc(C(=O)O)cc1
title compound
수율 90.3%
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccc(C(=O)O)cc1
4-Tri-n-butylstannylbenzoic acid
수율 90.3%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The resulting solution was refluxed for 2 hours
  2. 2
    온도The solution was cooled
  3. 3
    추출The solution was then extracted with diethyl ether (80 ml)
  4. 4
    세척The ether phase was washed with water (30 ml)
  5. 5
    건조dried over MgSO4 (5 g)
  6. 6
    여과filtered
  7. 7
    기타evaporated under reduced pressure

실험 절차

To a solution of methyl 4-tri-n-butylstannylbenzoate (3.0 g, 7 mmol) in absolute ethanol (60 ml) was added 0.25 g KOH (9 mmol). The resulting solution was refluxed for 2 hours. The solution was cooled and poured into an ice-cold solution of acetic acid (0.64 g, 10.6 mmol) and water (100 ml). The solution was then extracted with diethyl ether (80 ml). The ether phase was washed with water (30 ml), dried over MgSO4 (5 g), filtered and evaporated under reduced pressure to afford 2.6 g (88%) of the title compound. This material was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05746997uspto-grants-1998_05