Acetic Acid → HCID 178426257、化合物

HRID 1470226ノート

反応式

HRID 1470226 の反応式
[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

参加物

5

反応物 2

HCID 176Acetic Acid2 回HCID 443866Pemirolast potassium

生成物 1

HCID 178426257HCID 178426257、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cacbae007d554692bc90763df8954233
出典データセット
uspto-grants-2015_04
特許番号
US09006431B2

反応ノート

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