Acetic Acid → HCID 178426257, 화합물

HRID 1470226노트

반응식

HRID 1470226 반응식
[CH3:1][C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]3[N-:14][N:15]=[N:16][N:17]=3)[C:11](=[O:12])[N:6]2[CH:5]=[CH:4][CH:3]=1.[K+].C(O)(=O)C>O.C1COCC1>[CH3:1][C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]3[NH:14][N:15]=[N:16][N:17]=3)[C:11](=[O:12])[N:6]2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 176Acetic Acid2회HCID 443866Pemirolast potassium

생성물 1

HCID 178426257HCID 178426257, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

Pemirolast potassium (190 g; 0.71 mol; Chemtronica AB) was dissolved in a mixture of water (2,500 mL) and THF (1,400 mL) with stirring for 1 h at room temperature. The mixture was then clear-filtered, and acetic acid (43 g, 0.72 mol) in water (400 mL) was added in 2 portions. Firstly, approximately 50 mL of the mixture was added and the resultant slurry stirred for 30 minutes. Then, the rest of the acetic acid solution was added slowly. The resultant slurry was equilibrated over 2 hours, filtered and washed with water. The sub-title compound was air-dried overnight and then dried in a vacuum oven at 40° C. for 24 hours. The yield was 164 g (white solid, hard clumps).

후처리

  1. filtrationThe mixture was then clear-filtered
  2. stirringthe resultant slurry stirred for 30 minutes
  3. waitThe resultant slurry was equilibrated over 2 hours
  4. filtrationfiltered
  5. washwashed with water
  6. dry with materialThe sub-title compound was air-dried overnight
  7. customdried in a vacuum oven at 40° C. for 24 hours

출처 및 근거

ORD 기록
ord-cacbae007d554692bc90763df8954233
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006431B2

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