Acetic Acid → HCID 69003844, 화합물

HRID 225511노트

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HRID 225511 반응식
CO[CH2:3][CH2:4][O:5][CH3:6].[C:7](/[C:9](/[C:24]1[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=1)=[CH:10]\[N:11]([CH2:19][C:20]([O:22][CH3:23])=[O:21])CCC(OCC)=O)#[N:8].[CH2:30]1[CH2:40]CN2C(=NCCC2)CC1.C(O)(=[O:43])C>>[NH2:8][C:7]1[C:9]([C:24]2[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=2)=[C:10]([CH2:40][CH2:30][C:6]([O:5][CH2:4][CH3:3])=[O:43])[NH:11][C:19]=1[C:20]([O:22][CH3:23])=[O:21]

참가 물질

5

반응물 4

HCID 176Acetic AcidHCID 80711,2-DimethoxyethaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 23122145HCID 23122145, 화합물

생성물 1

HCID 69003844HCID 69003844, 화합물수율 70%

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온도
60 °C

실험 절차

To an ethylene glycol dimethyl ether (50 mL) solution of ethyl 3-{((1Z)-2-cyano-2-(3-pyridyl)vinyl)[(methoxycarbonyl)methyl]amino}propanate (6.236 g) was added 1,8-diazabicyclo[5,4,0]-7-undecene (3.590 g), and the mixture was stirred at 60° C. overnight. The reaction solution was cooled to room temperature and neutralized with acetic acid, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/5), to obtain the title compound (4.380 g, yield 70%). The NMR data and ESI/MS data of the compound are given below.

후처리

  1. distillationthe solvent was distilled off under reduced pressure
  2. customThe residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/5)

출처 및 근거

ORD 기록
ord-41352add16f3403abe5a7a49ecec2673
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557113B2

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