Acetic Acid → HCID 11337475, 화합물

HRID 1927183노트

반응식

HRID 1927183 반응식
[NH2:1][C:2]1[C:7]([NH:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:6][CH:5]=[C:4]([NH:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[N:3]=1.[C:23]([OH:26])(=[O:25])[CH3:24]>C(O)C>[C:23]([OH:26])(=[O:25])[CH3:24].[NH2:1][C:2]1[C:7]([NH:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:6][CH:5]=[C:4]([NH:14][CH2:15][C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)[N:3]=1

참가 물질

4

반응물 2

HCID 176Acetic Acid2회HCID 53276Flupirtine

생성물 1

HCID 11337475HCID 11337475, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
40 °C

실험 절차

Under nitrogen atmosphere 40 g of 2-amino-3-carbethoxyamino-6-(4-fluoro-benzylamino)-pyridine were dissolved in 1100 ml of Ethanol (90%) at 60° C. 8 g of acetic acid were dissolved in 200 ml of ethanol at 20° C. The mixture was cooled down to 40° C. While stirring the solution of acetic acid was added. The solution was filtered at 20° C. and crystallisation occurred while cooling the solution down to −15° C. for 24 h. The product was collected by filtration and dried at reduced pressure at room temperature for 12 h. As a result of drying 38.0 g white crystals of the product were obtained.

후처리

  1. additionwas added
  2. filtrationThe solution was filtered at 20° C.
  3. customcrystallisation
  4. temperaturewhile cooling the solution down to −15° C. for 24 h
  5. filtrationThe product was collected by filtration
  6. customdried at reduced pressure at room temperature for 12 h
  7. customAs a result
  8. dry with materialof drying 38.0 g white crystals of the product
  9. customwere obtained

출처 및 근거

ORD 기록
ord-099a0e0871cd403d9f817563497ffaf0
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183267B2

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