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Hydrochloric Acid → HCID 86704560, 화합물

HRID 1022430
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HRID 1022430 반응식
Cl[C:2]1[C:7]2[CH:8]=[CH:9][N:10]([CH2:11][CH3:12])[C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1.[OH-:14].[Na+].Cl>O1CCOCC1>[Cl:13][C:4]1[NH:3][C:2](=[O:14])[C:7]2[CH:8]=[CH:9][N:10]([CH2:11][CH3:12])[C:6]=2[CH:5]=1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86704559HCID 86704559, 화합물

생성물 1

HCID 86704560HCID 86704560, 화합물수율 32.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
160 °C

실험 절차

A microwave reaction vial was charged with 4,6-dichloro-1-ethyl-1H-pyrrolo[3,2-c]pyridine (200 mg, 0.930 mmol), a 2M aqueous sodium hydroxide solution (10 mL) and 1,4-dioxane (3 mL). The vial was sealed and then heated in the microwave at 160° C. for 30 min. At this time, the resulting mixture was acidified to pH 6.5 with a 4M aqueous hydrochloric acid solution and then concentrated in vacuo. The residue was diluted with ethanol. The solids were removed by filtration, and the filtrate was concentrated in vacuo. Flash chromatography (10/1 methylene chloride/methanol) afforded 6-chloro-1-ethyl-1,5-dihydro-pyrrolo[3,2-c]pyridine-4-one (60 mg, 32.8%). LC-MS calcd. for C9H9ClN2O [(M)+] 196, obsd. 196.9.

후처리

  1. customA microwave reaction
  2. customThe vial was sealed
  3. concentrationconcentrated in vacuo
  4. additionThe residue was diluted with ethanol
  5. customThe solids were removed by filtration
  6. concentrationthe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-7f3b7028ac86409e9095ea7037dc20bd
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722661B2

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