Water → HCID 67449886、化合物

HRID 1465816ノート

反応式

HRID 1465816 の反応式
C(N(CC)CC)C.[N+:8]([C:11]1[CH:16]=[CH:15][C:14]([N:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)=[CH:13][C:12]=1[NH2:23])([O-:10])=[O:9].[CH3:24][N:25]([CH3:29])[C:26](Cl)=[O:27].O>CN(C=O)C>[CH3:24][N:25]([CH3:29])[C:26]([N:20]1[CH2:19][CH2:18][N:17]([C:14]2[CH:15]=[CH:16][C:11]([N+:8]([O-:10])=[O:9])=[C:12]([NH2:23])[CH:13]=2)[CH2:22][CH2:21]1)=[O:27]

参加物

6

反応物 4

HCID 962WaterHCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 6021122-Nitro-5-(1-piperazinyl)aniline

生成物 1

HCID 67449886HCID 67449886、化合物収率 92.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Under a nitrogen atmosphere, triethylamine (0.546 g, 5.4 mmol) was added to 2-nitro-5-piperazin-1-yl-phenylamine (1.0 g, 4.5 mmol) in dry DMF (8 mL) and the mixture was cooled in an ice water bath. Dimethylcarbamyl chloride (0.581 g, 5.4 mmol) was added slowly to this reaction mixture via syringe and the mixture was brought up to room temperature and stirred overnight. After overnight stirring, the reaction mixture was slowly poured into cold water (100 mL) and stirred for 1 hour resulting in the solidification of the product. This was filtered, dried give the product, 4-(3-Amino-4-nitro-phenyl) -piperazine-1-carboxylic acid dimethylamide, as a yellow solid, 1.2 g (92.4% yield), which was used without any further purification.

後処理

  1. temperaturethe mixture was cooled in an ice water bath
  2. customwas brought up to room temperature
  3. stirringAfter overnight stirring
  4. stirringstirred for 1 hour
  5. customresulting in the solidification of the product
  6. filtrationThis was filtered
  7. customdried

出典と根拠

ORDレコード
ord-d0c354364eb0440da9eaafcab7cab5e5
出典データセット
uspto-grants-2015_04
特許番号
US08999993B2

反応ノート

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