Acetic Acid → HCID 178527899、化合物

HRID 631944

反応式

HRID 631944 の反応式
[Br:1][C:2]1C=C[C:5]2OCO[C:4]=2[C:3]=1C=O.[CH3:13][CH:14]([OH:16])[CH3:15].[NH2:17][C:18]1[CH:27]=[CH:26][C:21]2[NH:22][C:23](=[S:25])[NH:24][C:20]=2[CH:19]=1.[C:28](O)(=[O:30])C>>[Br:1][C:2]1[CH:3]=[C:4](/[CH:5]=[N:17]/[C:18]2[CH:27]=[CH:26][C:21]3[NH:22][C:23](=[S:25])[NH:24][C:20]=3[CH:19]=2)[C:13]2[O:30][CH2:28][O:16][C:14]=2[CH:15]=1

参加物

5

反応物 4

HCID 176Acetic AcidHCID 3776IsopropanolHCID 27340026-Amino-2-mercaptobenzimidazoleHCID 110316405-Bromo-1,3-benzodioxole-4-carboxaldehyde

生成物 1

HCID 178527899HCID 178527899、化合物収率 83%

実験手順

5-bromobenzo[d][1,3]dioxol-4-carbaldehyde (0.24 g, 1.05 mmol), IPA (4.8 ml), and 5-amino-1H-benzo[d]imidazole-2(3H)-thione (0.2 g, 1.21 mmol) were put in a 25 ml flask, and acetic acid (10 ml) was slowly added dropwise thereto while the mixture was stirred under nitrogen charging conditions, followed by stirring for 12 hours under reflux conditions. After that, the temperature of the mixture was lowered to room temperature, and the thus obtained solid was washed with methylene chloride and methanol, followed by filtering, thereby obtaining clean (E)-5-((6bromobenzo[d][1,3]dioxol-4-yl)methyleneamino)-1H-benzo[d]imidazole-2(3H)-thione at 83% yield.

後処理

  1. stirringby stirring for 12 hours under reflux conditions
  2. customwas lowered to room temperature
  3. washthe thus obtained solid was washed with methylene chloride and methanol
  4. filtrationby filtering

出典と根拠

ORDレコード
ord-4ae515f8bb65489f940b93c4b1570404
出典データセット
uspto-grants-2016_04
特許番号
US09321751B2

関連ノート

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