반응 #501139

ord-4ba52b66eb2749b1a4af39d6f8e88f11

반응 방정식

O=C(O)Cc1nn(Cc2nc3cc(C(F)(F)F)ccc3s2)c(=O)c2ccccc12
[4-oxo-(5-trifluoromethyl-benzothiazol-2-ylmethyl)-3,4-dihydro-phthalazin-1-yl]-acetic acid
OCCN(CCO)CCO
triethanolamine
O=C(O)Cc1nn(Cc2nc3cc(C(F)(F)F)ccc3s2)c(=O)c2ccccc12.OCCN(CCO)CCO
title compound
수율 86.9%
O=C(O)Cc1nn(Cc2nc3cc(C(F)(F)F)ccc3s2)c(=O)c2ccccc12.OCCN(CCO)CCO
[4-Oxo-(5-trifluoromethyl-benzothiazol-2-ylmethyl)-3,4-dihydro-phthalazin-1-yl]-acetic Acid Triethanolamine Salt
수율 86.9%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the mixture was evaporated to a semi-solid, which
  2. 2
    기타was crystallized from ethanol:acetone (1:4)

실험 절차

To a solution of [4-oxo-(5-trifluoromethyl-benzothiazol-2-ylmethyl)-3,4-dihydro-phthalazin-1-yl]-acetic acid (419 mg, 1.0 mmol) in acetone (20 mL) was added triethanolamine (1.49 g, 10.0 mmol). After stirring at ambient temperature for 1.0 hours, the mixture was evaporated to a semi-solid, which was crystallized from ethanol:acetone (1:4) to afford the title compound as a white crystalline solid (494 mg, 86%). mp: 83-84° C.; 1H NMR (D2O, 350 MHz): δ 3.30 (m, 6H), 3.67 (s, 2H), 3.79 (m, 6H), 5.47 (s, 2H), 7.17 (m, 1H), 7.48-7.71 (m, 5H), 8.01 (m, 1H); MS (Cl) 419 (MH).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06570013B2uspto-grants-2003_05