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Hydrochloric Acid → HCID 118308737, 화합물

HRID 923520
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HRID 923520 반응식
[F:1][C:2]1[CH:36]=[CH:35][CH:34]=[C:33]([F:37])[C:3]=1[CH2:4][O:5][C:6]1[C:7]2[N:8]([C:12]([C:16]([NH:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH:26]3[CH2:30][O:29]C(C)(C)[O:27]3)=[O:17])=[C:13]([CH3:15])[N:14]=2)[CH:9]=[CH:10][CH:11]=1.O1CCOCC1.Cl.C(=O)([O-])O.[Na+]>CO>[F:1][C:2]1[CH:36]=[CH:35][CH:34]=[C:33]([F:37])[C:3]=1[CH2:4][O:5][C:6]1[C:7]2[N:8]([C:12]([C:16]([NH:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH:26]([OH:27])[CH2:30][OH:29])=[O:17])=[C:13]([CH3:15])[N:14]=2)[CH:9]=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 901926008-[(2,6-difluorobenzyl)oxy]-N-[2-(2,2-dimethyl-1,3-dioxolan-4-yl)benzyl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide

생성물 1

HCID 118308737HCID 118308737, 화합물수율 93.9%

시약·촉매·용매 1

HCID 887
Methanol
용매

실험 절차

To a mixture of 273 mg of 8-[(2,6-difluorobenzyl)oxy]-N-[2-(2,2-dimethyl-1,3-dioxolan-4-yl)benzyl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide, 3 ml of dioxane, and 3 ml of methanol was added 6 ml of 1 M hydrochloric acid under ice-cooling, followed by stirring at room temperature for 16 hours. The reaction mixture was ice-cooled and 0.6 g of sodium hydrogen carbonate was added thereto in small portions to make the mixture weakly basic. The precipitated solid was collected by filtration and washed with water to obtain 236 mg of 8-[(2,6-difluorobenzyl)oxy]-N-[2-(1,2-dihydroxyethyl)benzyl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide.

후처리

  1. temperaturecooling
  2. temperaturecooled
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water

출처 및 근거

ORD 기록
ord-ceb4012737444af0929b49d6ae1a6e0e
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278968B2

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