Water → HCID 90411819、化合物

HRID 1850696ノート

反応式

HRID 1850696 の反応式
[H-].[Na+].[Br:3][C:4]1[C:5]([CH3:10])=[N:6][S:7][C:8]=1N.[NH2:11][C:12]1[C:21]([C:22]([O:24]N2C3C=C(Cl)C=CC=3N=N2)=[O:23])=[C:15]2[N:16]=[CH:17][C:18]([F:20])=[CH:19][N:14]2[N:13]=1.O>CN1C(=O)CCC1>[NH2:11][C:12]1[C:21]([C:22]([O:24][C:8]2[S:7][N:6]=[C:5]([CH3:10])[C:4]=2[Br:3])=[O:23])=[C:15]2[N:16]=[CH:17][C:18]([F:20])=[CH:19][N:14]2[N:13]=1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 177499314-Bromo-3-methyl-1,2-thiazol-5-amineHCID 86720889HCID 86720889、化合物

生成物 1

HCID 90411819HCID 90411819、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

NaH (210.3 mg, 5.259 mmol) was added to a solution of 4-bromo-3-methyl-isothiazol-5-amine (533 mg, 2.761 mmol) in dry NMP (21.95 mL) at RT. The solution was stirred at RT for 5 min before (6-chlorobenzotriazol-1-yl) 2-amino-6-fluoro-pyrazolo[1,5-a]pyrimidine-3-carboxylate 6a* (914.4 mg, 2.630 mmol) was added. After 10 min, the reaction mixture was treated with water (120 mL) and stirred for 15 mins. The pale brown solid was filtered off and dried in vacuo to afford 4-bromo-3-methylisothiazol-5-yl 2-amino-6-fluoropyrazolo[1,5-a]pyrimidine-3-carboxylate. (801 mg, 82%). MS (ES+) 370.5.

後処理

  1. additionwas added
  2. filtrationThe pale brown solid was filtered off
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-4912994b3abc4374bbf0f163990528c3
出典データセット
uspto-grants-2015_02
特許番号
US08957078B2

反応ノート

読み込み中…