Sodium Nitrite → HCID 178518865、化合物

HRID 30412ノート

反応式

HRID 30412 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][NH:9][C:10](=[O:19])[C:11]1[C:16]([F:17])=[CH:15][CH:14]=[CH:13][C:12]=1N.N([O-])=O.[Na+]>Cl.O.CCO.O>[F:17][C:16]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:11]=1[C:10]([OH:19])=[N:9][N:8]2[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[F:1]

参加物

6

反応物 2

HCID 23668193Sodium NitriteHCID 685283982-amino-6-fluoro-benzoic acid N'-(2-fluoro-phenyl)-hydrazide

生成物 1

HCID 178518865HCID 178518865、化合物収率 95%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 19096565Water ethanol溶媒

反応条件

温度
0 °C

実験手順

Intermediate 44 (2.182 g, 8.289 mmol) was suspended in 1M HCl (20 ml), cooled to 0° C. and treated dropwise with a solution of sodium nitrite (1.144 g, 16.58 mmol) in water (7 ml). The mixture was stirred for 10 minutes at 0° C., diluted with 1:1 EtOH/H2O (30 ml) and heated to reflux for 3 hours, then stirred at room temperature for 18 hours. The solid was filtered, rinsed with water and dried to afford 1.939 g (95%) of 4-fluoro-1-(2-fluoro-phenyl)-1H-indazol-3-ol (Intermediate 45) as a tan solid. MS (APCI): (M+1)=247.1, (M−1)=245.0.

後処理

  1. temperatureheated
  2. temperatureto reflux for 3 hours
  3. stirringstirred at room temperature for 18 hours
  4. filtrationThe solid was filtered
  5. washrinsed with water
  6. customdried

出典と根拠

ORDレコード
ord-42ec122c690144d88b4a34901f72d5a9
出典データセット
uspto-grants-2008_09
特許番号
US07423054B2

反応ノート

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