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Hydrochloric Acid → HCID 22142147、化合物

HRID 1824696
ノート
印刷プレビュー

反応式

HRID 1824696 の反応式
Cl.[F:2][C:3]1[CH:4]=[C:5]([NH:20][NH2:21])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=1.N1C=CC=CC=1.[C:28](Cl)(=[O:30])[CH3:29].Cl>C(OCC)(=O)C.O>[F:2][C:3]1[CH:4]=[C:5]([NH:20][NH:21][C:28](=[O:30])[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6367Acetyl chlorideHCID 22142154HCID 22142154、化合物

生成物 1

HCID 22142147HCID 22142147、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857
Ethyl Acetate
溶媒

実験手順

To [3-fluoro-4-[3-(trifluoromethyl)phenoxy]phenyl]hydrazine hydrochloride (0.35 g) prepared using the method described in Example 1, in ethyl acetate (5 mL), was added pyridine (0.24 mL) at −10° C. After dropwise addition of acetyl chloride (0.1 mL), the mixture was stirred for 3 h and then acidified with 6 M HCl. Water was added, and the product was extracted with ether. The organic layer was separated, dried, and concentrated. The residue was purified by column chromatography on silica (using dichloromethane, followed by 5:1 dichloromethane:ether as eluants) to give a solid (0.2 g).

後処理

  1. extractionthe product was extracted with ether
  2. customThe organic layer was separated
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on silica (using dichloromethane, followed by 5:1 dichloromethane:ether as eluants)

出典と根拠

ORDレコード
ord-8d75ea7c051b451ca8495733475d3360
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07045512B2

反応ノート

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