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Potassium Carbonate → 2-[3-(4-chlorophenyl)-4-(3-fluorophenylmethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-N-[3-(tri-fluoromethyl)phenylmethyl]acetamide

HRID 660928
ノート
印刷プレビュー

反応式

HRID 660928 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[CH:16]=3)[C:10](=[O:13])[NH:11][N:12]=2)=[CH:4][CH:3]=1.Cl[CH2:23][C:24]([NH:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([C:34]([F:37])([F:36])[F:35])[CH:29]=1)=[O:25].C(=O)([O-])[O-].[K+].[K+]>C(#N)C.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[CH:16]=3)[C:10](=[O:13])[N:11]([CH2:23][C:24]([NH:26][CH2:27][C:28]3[CH:33]=[CH:32][CH:31]=[C:30]([C:34]([F:35])([F:36])[F:37])[CH:29]=3)=[O:25])[N:12]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 212778322-Chloro-N-(3-trifluoromethyl-benzyl)-acetamideHCID 580118615-(4-chlorophenyl)-4-(3-fluorophenylmethyl)-2,4-dihydro-3H-1,2,4-triazol-3-one

生成物 1

HCID 580122682-[3-(4-chlorophenyl)-4-(3-fluorophenylmethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-N-[3-(tri-fluoromethyl)phenylmethyl]acetamide

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6342Acetonitrile溶媒

実験手順

200 mg (0.66 mmol) of 5-(4-chlorophenyl)-4-(3-fluorophenylmethyl)-2,4-dihydro-3H-1,2,4-triazol-3-one from Example 41A, 193 mg (0.69 mmol) of 2-chloro-N-[3-(trifluoromethyl)phenylmethyl]-acetamide [preparable according to EP 0 163 607, Example 28] and 182 mg (1.32 mmol) of potassium carbonate are suspended in 2.5 ml of acetonitrile and heated under reflux overnight. After cooling, this is diluted with water, and purified by preparative HPLC [Method 9] and 219 mg (64% of theory) of the target compound are thus obtained.

後処理

  1. temperatureheated
  2. temperatureunder reflux overnight
  3. temperatureAfter cooling
  4. custompurified by preparative HPLC [Method 9] and 219 mg (64% of theory) of the target compound
  5. customare thus obtained

出典と根拠

ORDレコード
ord-e9fb8c98335f4cecba95ab0526f95e07
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084481B2

反応ノート

読み込み中…

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