Formic Acid → HCID 178432647, 화합물

HRID 1047294노트

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HRID 1047294 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:9](=[NH:12])[NH:10][NH2:11])=[N:6][C:7]=1[CH3:8].[CH:13](O)=O>CO>[Br:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([C:9]2[NH:12][CH:13]=[N:11][N:10]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 284Formic AcidHCID 178432964HCID 178432964, 화합물

생성물 1

HCID 178432647HCID 178432647, 화합물수율 84%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
100 °C

실험 절차

5-Bromo-6-methylpicolin-imido-hydrazide (1 equiv) and formic acid (15 equiv) were combined and heated with stirring at 100° C. for 6 h. The reaction was cooled to room temperature and diluted with methanol. The resulting slurry was stirred for 30 min and then partially concentrated under reduced pressure to ˜20% of the total volume. The resulting mixture was again diluted with methanol and partially concentrated under reduced pressure to ˜20% of the total volume. The resulting solids were collected by filtration, washed three times with water and dried under reduced pressure to provide the desired product in 84% yield, as an off-white solid. MS (ESI) m/z 238.9 [M]+, 240.9 [M+2]+.

후처리

  1. temperatureheated
  2. temperatureThe reaction was cooled to room temperature
  3. stirringThe resulting slurry was stirred for 30 min
  4. concentrationpartially concentrated under reduced pressure to ˜20% of the total volume
  5. additionThe resulting mixture was again diluted with methanol
  6. concentrationpartially concentrated under reduced pressure to ˜20% of the total volume
  7. filtrationThe resulting solids were collected by filtration
  8. washwashed three times with water
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-cc9e6d97fb434aa5b040808254e08e42
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569494B2

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