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Hydrochloric Acid → HCID 16225331, 화합물

HRID 390601
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HRID 390601 반응식
[ClH:1].[CH2:2]([O:4]/[C:5](=[CH:9]\[C:10]1[CH:11]=[N:12][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([N:22]([CH3:33])[C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[O:24])[CH:17]=2)=[CH:14][CH:15]=1)/[C:6]([OH:8])=[O:7])[CH3:3]>C(O)C>[ClH:1].[CH2:2]([O:4]/[C:5](=[CH:9]\[C:10]1[CH:11]=[N:12][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([N:22]([CH3:33])[C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[O:24])[CH:17]=2)=[CH:14][CH:15]=1)/[C:6]([OH:8])=[O:7])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 16225332HCID 16225332, 화합물

생성물 1

HCID 16225331HCID 16225331, 화합물수율 77%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.3 mL (0.3 mmol) of a 1 N ethanolic hydrogen chloride solution is added to a solution of 0.12 g (0.3 mmol) of (Z)-2-ethoxy-3-{6-[3-(3-heptyl-1-methylureido)phenyl]pyrid-3-yl}acrylic acid in 1 mL of ethanol, precooled to 0° C. The ethanol is evaporated off under a flow of nitrogen and 6 mL of diethyl ether are added. The hydrochloride precipitates; the reaction medium is filtered off and the solid obtained is rinsed thoroughly with diethyl ether. The solid obtained is recrystallized from a hot mixture of acetone and a minimum amount of water. 100 mg (77%) of (Z)-2-ethoxy-3-{6-[3-(3-heptyl-1-methylureido)phenyl]pyrid-3-yl}acrylic acid hydrochloride are obtained in the form of a yellow solid with a melting point of 170° C.

후처리

  1. customprecooled to 0° C
  2. customThe ethanol is evaporated off under a flow of nitrogen and 6 mL of diethyl ether
  3. additionare added
  4. customThe hydrochloride precipitates
  5. filtrationthe reaction medium is filtered off
  6. customthe solid obtained
  7. washis rinsed thoroughly with diethyl ether
  8. customThe solid obtained
  9. customis recrystallized from a hot mixture of acetone

출처 및 근거

ORD 기록
ord-3b9e7c763bc942baa50923268845f4f8
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383652B2

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