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Triethylamine → HCID 69506730, 화합물

HRID 2366667
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HRID 2366667 반응식
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([C:11]=1[NH:12][CH2:13][C:14]([CH3:21])([CH3:20])[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:9][CH:8]=[CH:7][CH:6]=2.[CH2:22]([O:24][CH2:25][C:26](Cl)=O)[CH3:23].C(N(CC)CC)C>C(O)C>[CH2:22]([O:24][CH2:25][C:26]1[N:12]([CH2:13][C:14]([CH3:20])([CH3:21])[C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:11]2[C:10]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:4]=[CH:3][C:2]=2[N:1]=1)[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471Triethylamine2회HCID 84189Ethoxyacetyl chloride2회HCID 57447056HCID 57447056, 화합물

생성물 1

HCID 69506730HCID 69506730, 화합물수율 36.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A modification of the method described in Part C of Example 5 was used to treat ethyl 3-[(3-aminoquinolin-4-yl)amino]-2,2-dimethylpropanoate (15.5 g, 60.2 mmol, prepared in Parts A through D of Example 26) with ethoxyacetyl chloride (8.7 g, 71 mmol) followed by triethylamine (24.4 mL, 175 mmol). The reaction with ethoxyacetyl chloride was stirred overnight, and the reaction with triethylamine was heated at reflux in ethanol (125 mL) for four days. Following the work-up procedure, the crude product was purified by column chromatography on silica gel (eluting with dichloromethane:methanol in a gradient from 100:0 to 95:5) to provide 7.9 g of ethyl 3-[2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-1-yl]-2,2-dimethylpropanoate as an oil.

후처리

  1. temperaturewas heated
  2. customthe crude product was purified by column chromatography on silica gel (
  3. washeluting with dichloromethane

출처 및 근거

ORD 기록
ord-21427562f4514c5c985c0024340f59de
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697873B2

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