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1,2-Dichloroethane → HCID 178447333、化合物

HRID 1258750
ノート
印刷プレビュー

反応式

HRID 1258750 の反応式
[N:1]([C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][C:17]=1[O:18][C:19]([F:22])([F:21])[F:20])[CH2:7][NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[C:2]=S.[NH2:23][C:24]1[C:31]([NH2:32])=[CH:30][C:27]([C:28]#[N:29])=[C:26]([N:33]2[CH2:38][CH2:37][CH2:36][CH:35]([C:39]([F:42])([F:41])[F:40])[CH2:34]2)[CH:25]=1.CN(C=O)C.C(Cl)CCl>C(Cl)(Cl)Cl.O>[C:28]([C:27]1[C:26]([N:33]2[CH2:38][CH2:37][CH2:36][CH:35]([C:39]([F:42])([F:40])[F:41])[CH2:34]2)=[CH:25][C:24]2[NH:23][C:2]([NH:1][C:4]3[CH:5]=[C:6]([CH:15]=[CH:16][C:17]=3[O:18][C:19]([F:22])([F:21])[F:20])[CH2:7][NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[N:32][C:31]=2[CH:30]=1)#[N:29]
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 111,2-DichloroethaneHCID 6228DimethylformamideHCID 679577914,5-Diamino-2-(3-trifluoromethyl-piperidin-1-yl)benzonitrileHCID 86674354N-(3-Isothiocyanato-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide

生成物 1

HCID 178447333HCID 178447333、化合物

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6212Chloroform溶媒

実験手順

A mixture of N-(3-isothiocyanato-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide (135 mg, 0.406 mmol), 4,5-diamino-2-(3-trifluoromethyl-piperidin-1-yl)benzonitrile (115 mg, 0.406 mmol) and DMF (2 mL) was stirred at rt for 4 h. EDC (101 mg, 0.527 mmol) was added and mixture was stirred at rt overnight. The mixture was treated with water and extracted with Et2O. Concentration and purification by column chromatography gave an oil. The oil was treated with CHCl3 and the precipitate was collected by filtration.

後処理

  1. stirringmixture was stirred at rt overnight
  2. extractionextracted with Et2O
  3. concentrationConcentration and purification by column chromatography
  4. customgave an oil
  5. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-1ca4f1d92d9d43c5be95592e6fc7dbab
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08466186B2

反応ノート

読み込み中…

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