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Water → HCID 25110856, 화합물

HRID 751543
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HRID 751543 반응식
F[C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].Cl[CH2:13][CH2:14][O:15][C:16](Cl)=[O:17].[CH3:19][O-:20].[Na+].O>CN1CCCC1=O>[CH3:19][O:20][C:2]1[CH:8]=[CH:7][C:5]([N:6]2[CH2:13][CH2:14][O:15][C:16]2=[O:17])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10]
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참가 물질

6

반응물 4

HCID 962WaterHCID 123052-Chloroethyl chloroformateHCID 677684-Fluoro-3-nitroanilineHCID 10942334Sodium Methoxide

생성물 1

HCID 25110856HCID 25110856, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

4-Fluoro-3-nitro-aniline (50.0 g) is dissolved in 100 ml N-methyl-pyrrolidone. Subsequently 2-chloroethyl-chloroformate (48.1 g) is added dropwise under external cooling, whereupon the internal temperature is kept below 60° C. After completion of the addition stirring is continued for 30 minutes and then a 30% methanolic sodium methoxide solution (230.7 g) is added dropwise in such a rate that under external cooling the temperature remains below 40° C. When the addition is completed, the reaction mixture is allowed to cool and then poured into cold water (2000 ml) and stirred for additional 30 minutes. The obtained suspension is filtered off, washed with water, and dried.

후처리

  1. customis kept below 60° C
  2. additionAfter completion of the addition
  3. temperatureunder external cooling the temperature
  4. customremains below 40° C
  5. additionWhen the addition
  6. temperatureto cool
  7. stirringstirred for additional 30 minutes
  8. filtrationThe obtained suspension is filtered off
  9. washwashed with water
  10. customdried

출처 및 근거

ORD 기록
ord-2d1a79f5acb748b5acb519668313ef0e
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07405325B2

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