Water → HCID 67449886, 화합물

HRID 1465816노트

반응식

HRID 1465816 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 67449886HCID 67449886, 화합물수율 92.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d0c354364eb0440da9eaafcab7cab5e5
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999993B2

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