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3-(Trifluoromethyl)benzaldehyde → N*3*-(3,5-Dichloro-phenyl)-N*5*-(3-trifluoromethyl-benzyl)-1H-[1,2,4]triazole-3,5-diamine

HRID 1486590
ノート
印刷プレビュー

反応式

HRID 1486590 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[N:14]=[C:13]([NH2:15])[NH:12][N:11]=2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.ClC1C=C(N=C=S)C=C(Cl)C=1C#N.[F:29][C:30]([F:40])([F:39])[C:31]1[CH:32]=[C:33]([CH:36]=[CH:37][CH:38]=1)[CH:34]=O.[BH4-].[Na+]>CO.O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[N:14]=[C:13]([NH:15][CH2:34][C:33]3[CH:36]=[CH:37][CH:38]=[C:31]([C:30]([F:29])([F:39])[F:40])[CH:32]=3)[NH:12][N:11]=2)[CH:5]=[C:6]([Cl:8])[CH:7]=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 679903-(Trifluoromethyl)benzaldehydeHCID 4311764Sodium borohydrideHCID 727146143-Amino-5-(3,5-dichloroanilino)-s-triazoleHCID 867076002,6-Dichloro-4-isothiocyanatobenzonitrile

生成物 1

HCID 178506159N*3*-(3,5-Dichloro-phenyl)-N*5*-(3-trifluoromethyl-benzyl)-1H-[1,2,4]triazole-3,5-diamine収率 46%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 962Water溶媒

実験手順

To a stirred solution of N3-(3,5-dichlorophenyl)-1H-1,2,4-triazole-3,5-diamine Intermediate 2 (80 mg, 0.33 mmol) in 5 mL methanol, was added 3-(trifluoromethyl)benzaldehyde (114 mg, 0.66 mmol). The reaction mixture was stirred overnight, after which, sodium borohydride (24.8 mg, 0.656 mmol) was added and the mixture was for stirred for 10 min. The reaction was diluted the water (20 mL) and extracted with EtOAc (3×10 mL). The organic layers were combined and dried with sodium sulfate. The solvent was removed and the residue was chromatographed on a combiflash machine (6% methanol/methylene chloride) to give 61 mg (46%) of the desired product. MS +m/z: 401.9 (M+H)+

後処理

  1. stirringfor stirred for 10 min
  2. extractionextracted with EtOAc (3×10 mL)
  3. dry with materialdried with sodium sulfate
  4. customThe solvent was removed
  5. customthe residue was chromatographed on a combiflash machine (6% methanol/methylene chloride)

出典と根拠

ORDレコード
ord-9aa7630a2cf248acb1e0611c9635ae49
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428469B2

反応ノート

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