Formic Acid → HCID 178432647, 화합물

HRID 2200323노트

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HRID 2200323 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, 화합물

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 to 100° C. for 6 h. The reaction was cooled to room temperature and diluted with methanol. The resulting slurry was partially concentrated under reduced pressure and the resulting mixture was diluted with methanol and partially concentrated under reduced pressure. The resulting solids were collected by filtration, washed with water and dried to provide the desired product, as a solid. MS (ESI) m/z 238.9 [M]+, 240.9 [M+2]+.

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. concentrationThe resulting slurry was partially concentrated under reduced pressure
  3. additionthe resulting mixture was diluted with methanol
  4. concentrationpartially concentrated under reduced pressure
  5. filtrationThe resulting solids were collected by filtration
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-91ba00941eff47dd9f320718d2efa8dd
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359364B2

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