Lithium hydroxide, monohydrate → HCID 22918423、化合物

HRID 1376759ノート

反応式

HRID 1376759 の反応式
C[O:2][C:3](=[O:30])[C:4]1[C:5](=[CH:10][C:11]([NH:22][C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)=[C:12]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[CH:13]=1)[C:6]([O:8]C)=[O:7].O.[OH-].[Li+]>CO.O>[F:21][C:18]1[CH:19]=[CH:20][C:15]([NH:14][C:12]2[CH:13]=[C:4]([C:3]([OH:30])=[O:2])[C:5](=[CH:10][C:11]=2[NH:22][C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[C:6]([OH:8])=[O:7])=[CH:16][CH:17]=1

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 10476762HCID 10476762、化合物

生成物 1

HCID 22918423HCID 22918423、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

A steady stream of argon is passed through a suspension of 5.0 g (12.12 mmol) of 4,5-bis-(4-fluoroanilino)phthalic acid dimethylester in 40 ml of methanol, and a solution of 2.04 g (48.6 mmol, 2 eq) of lithium hydroxide monohydrate in 20 ml of water is added. The reaction mixture is heated to reflux for 1 hour, cooled to RT and diluted with 50 ml water. Methanol is removed by evaporation, the resulting solution is cooled to 0°, and 12 ml 4N hydrochloric acid and thereafter 100 ml of water are added. After 15 rain at 0°, the gray crystals are filtered off, washed with water and resuspended twice in 100 ml toluene with removal of the toluene by distillation to yield the title compound in the form of gray crystals, FAB-MS: 385 [M+ +H].

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for 1 hour
  3. customMethanol is removed by evaporation
  4. temperaturethe resulting solution is cooled to 0°
  5. addition12 ml 4N hydrochloric acid and thereafter 100 ml of water are added
  6. filtrationAfter 15 rain at 0°, the gray crystals are filtered off
  7. washwashed with water
  8. customresuspended twice in 100 ml toluene with removal of the toluene by distillation

出典と根拠

ORDレコード
ord-7654b146ca544f2ca3e1c4b1d199436e
出典データセット
uspto-grants-1997_09
特許番号
US05663336

反応ノート

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