Tetomilast → HCID 86645102、化合物

HRID 1888930ノート

反応式

HRID 1888930 の反応式
[CH3:1][CH2:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([C:13]2[S:17][CH:16]=[C:15]([C:18]3[CH:19]=[CH:20][CH:21]=[C:22]([C:24]([OH:26])=[O:25])[N:23]=3)[N:14]=2)=[CH:8][C:9]=1[O:10][CH2:11][CH3:12]>C(#N)C>[CH3:1][CH2:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([C:13]2[S:17][CH:16]=[C:15]([C:18]3[CH:19]=[CH:20][CH:21]=[C:22]([C:24]([OH:26])=[O:25])[N:23]=3)[N:14]=2)=[CH:8][C:9]=1[O:10][CH2:11][CH3:12].[C:13](#[N:14])[CH3:7]

参加物

3

反応物 1

HCID 3025803Tetomilast

生成物 1

HCID 86645102HCID 86645102、化合物収率 183.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
30 °C

実験手順

5 g of the anhydrous tetomilast type A crystal obtained in Example 1 (6) was dissolved in 400 ml of acetonitrile, while stirring under heating to reflux. The obtained solution was cooled to approximately 30° C. over about 1 hour, and it was then further cooled at 10° C. or lower for 1 hour, so as to obtain the precipitated crystal by filtration. The above precipitated crystal was dried at 50° C. for 3 hours, so as to obtain 5.1 g of a tetomilast acetonitrile solvate crystal in the form of a while platy crystal (yield: quantitative).

後処理

  1. temperatureunder heating to reflux
  2. temperatureit was then further cooled at 10° C. or lower for 1 hour
  3. customso as to obtain the precipitated crystal
  4. filtrationby filtration
  5. customThe above precipitated crystal
  6. customwas dried at 50° C. for 3 hours

出典と根拠

ORDレコード
ord-9f7b97f96a05417dbeefc1c91e0e008e
出典データセット
uspto-grants-2013_08
特許番号
US08501949B2

反応ノート

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