Bromine → HCID 178510531、化合物

HRID 1993821

反応式

HRID 1993821 の反応式
[C:1]([CH:3]([C:7](=[S:25])[NH:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][C:16]2[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=2[Cl:23])=[C:11]([F:24])[CH:10]=1)[C:4]([NH2:6])=[O:5])#[N:2].BrBr>C(OCC)(=O)C>[Cl:23][C:17]1[CH:18]=[CH:19][C:20]([Cl:22])=[CH:21][C:16]=1[O:15][C:12]1[CH:13]=[CH:14][C:9]([NH:8][C:7]2[S:25][N:6]=[C:4]([OH:5])[C:3]=2[C:1]#[N:2])=[CH:10][C:11]=1[F:24]

参加物

4

反応物 2

HCID 24408BromineHCID 597977082-Cyano-2-[4-(2,5-dichloro-phenoxy)-3-fluoro-phenylthiocarbamoyl]-acetamide

生成物 1

HCID 178510531HCID 178510531、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

2-Cyano-2-[4-(2,5-dichloro-phenoxy)-3-fluoro-phenylthiocarbamoyl]-acetamide (1.6 g, 4 mmol) was dissolved in anhydrous ethyl acetate (60 ml) and a solution of bromine (0.2 ml, 4 mmol) in anhydrous ethyl acetate (10 ml) was added dropwise into the mixture with stirring at room temperature. After addition, the reaction mixture was stirred for another 3 hours. The precipitate was filtered and the solid was washed with ethyl ether and suspended in a saturated sodium bicarbonate with stirring for 10 min. The solid was filtered, then washed with water and dried in vacuo to afford a white powder.

後処理

  1. additionAfter addition
  2. stirringthe reaction mixture was stirred for another 3 hours
  3. filtrationThe precipitate was filtered
  4. washthe solid was washed with ethyl ether
  5. stirringwith stirring for 10 min
  6. filtrationThe solid was filtered
  7. washwashed with water
  8. customdried in vacuo
  9. customto afford a white powder

出典と根拠

ORDレコード
ord-7d752b218a7a4891947964a1a7ef3a59
出典データセット
uspto-grants-2010_01
特許番号
US07652047B2

関連ノート

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