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Methyl iodide → HCID 178470168, 화합물

HRID 2093064
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HRID 2093064 반응식
[NH:1]([C:8]([N:10]1[CH2:15][CH2:14][C:13]2[N:16]=[C:17]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[S:18][C:12]=2[CH2:11]1)=[S:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:24]([O-])([O-])=O.[K+].[K+].IC>CC(C)=O>[CH3:24][S:9]/[C:8](=[N:1]\[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)/[N:10]1[CH2:15][CH2:14][C:13]2[N:16]=[C:17]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[S:18][C:12]=2[CH2:11]1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86650190Ethyl 5-(anilinocarbonothioyl)-4,5,6,7-tetrahydro[1,3]thiazolo[5,4-c]pyridine-2-carboxylate

생성물 1

HCID 178470168HCID 178470168, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of ethyl 5-(anilinocarbonothioyl)-4,5,6,7-tetrahydro[1,3]thiazolo[5,4-c]pyridine-2-carboxylate obtained in step I (1 eq) in acetone, K2CO3 (1.2 eq) was added and the reaction mixture was stirred for 15 min. To this, iodomethane (1.2 eq) was added and the reaction was continued at room temperature for 5 h. Solvent was evaporated and the residue was diluted dichloromethane. It was then washed with water and the organic layer was separated, dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford crude product, which, on purification by column chromatography afforded the ethyl 5-[(Z)(methylthio)(phenylimino)methyl]-4,5,6,7-tetrahydro[1,3]thiazolo[5,4-c]pyridine-2-carboxylate.

후처리

  1. waitthe reaction was continued at room temperature for 5 h
  2. customSolvent was evaporated
  3. washIt was then washed with water
  4. customthe organic layer was separated
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customto afford crude product, which
  8. customon purification by column chromatography

출처 및 근거

ORD 기록
ord-520c620d4e254cb5bcc05c50752b19f8
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08440830B2

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