Formic Acid → HCID 19605204, 화합물

HRID 1603504노트

반응식

HRID 1603504 반응식
[CH:1]([OH:3])=O.C(OC(=O)C)(=O)C.[NH2:11][CH2:12][C:13]1[N:14]2[CH:21]=[N:20][CH:19]=[C:15]2[S:16][C:17]=1[CH3:18].C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH:1]([NH:11][CH2:12][C:13]1[N:14]2[CH:21]=[N:20][CH:19]=[C:15]2[S:16][C:17]=1[CH3:18])=[O:3]

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 19605190HCID 19605190, 화합물

생성물 1

HCID 19605204HCID 19605204, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 0.94 ml of formic acid and 0.47 ml of acetic anhydride which had been beforehand reacted with each other at 50° C. for 30 minutes was added at room temperature to 5 ml of a dry dichloromethane solution containing 167 mg of 3-aminomethyl-2-methylimidazo[5,1-b]thiazole, and the mixture was then stirred at the same temperature for 1 hour. Then, an aqueous potassium carbonate solution was added to the reaction solution to alkalify the same. The organic layer was separated, and the aqueous layer was further extracted five times with dichloromethane. The combined organic layer was dried over anhydrous sodium sulfate and then filtered, and the solvent was evaporated under reduced pressure to obtain 117 mg of the title compound.

후처리

  1. customhad been beforehand reacted with each other at 50° C. for 30 minutes
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was further extracted five times with dichloromethane
  4. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-26b055f045934938b987753b0a4448cc
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990101

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