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Water → HCID 22273086, 화합물

HRID 1064365
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인쇄 미리보기

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HRID 1064365 반응식
[Cl:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[C:5]([NH2:6])=[C:4]([F:12])[C:3]=1F.[N:14]1([CH2:20][CH2:21][OH:22])[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[Cl:1][C:2]1[C:3]([N:17]2[CH2:18][CH2:19][N:14]([CH2:20][CH2:21][OH:22])[CH2:15][CH2:16]2)=[C:4]([F:12])[C:5]([NH2:6])=[C:7]([N+:9]([O-:11])=[O:10])[CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 76771-(2-Hydroxyethyl)piperazineHCID 11430Potassium CarbonateHCID 178973294-Chloro-2,3-difluoro-6-nitroaniline

생성물 1

HCID 22273086HCID 22273086, 화합물수율 67.3%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
50 °C

실험 절차

To a solution of 6.79 g of 4-chloro-2,3-difluoro-6-nitroaniline (which was synthesized following WO9856761 or WO9835977) and 4.70 g of 1-piperazine ethanol in 30 ml of dimethylsulfoxide, 9.23 g of potassium carbonate was added, followed by an hour's stirring at 50° C. After cooling the reaction liquid to room temperature, water was added thereto, followed by extraction with chloroform. The chloroform layer was dried on anhydrous magnesium sulfate, the solvent was distilled off and 6.98 g of the title compound in crude form was obtained as a yellow oily substance.

후처리

  1. waitfollowed by an hour
  2. temperatureAfter cooling
  3. customthe reaction liquid to room temperature
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe chloroform layer was dried on anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-dd8929cfcc57458f93f3ea05beea15bc
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06969712B2

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