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Acetic Acid → HCID 21226443, 화합물

HRID 583048
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HRID 583048 반응식
C(O)(=O)C.[Cl:5][C:6]1[C:7]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[C:18]([N+:23]([O-])=O)[CH:17]=2)=[N:8][N:9]([CH3:15])[C:10]=1[O:11][CH:12]([F:14])[F:13].C(OCC)(=O)C>C(O)C.[Fe]>[NH2:23][C:18]1[CH:17]=[C:16]([C:7]2[C:6]([Cl:5])=[C:10]([O:11][CH:12]([F:13])[F:14])[N:9]([CH3:15])[N:8]=2)[CH:21]=[CH:20][C:19]=1[Cl:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 8857Ethyl AcetateHCID 21226452HCID 21226452, 화합물

생성물 1

HCID 21226443HCID 21226443, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

155 ml of acetic acid were added to a suspension of 32.1 g (0.576 mol) of iron powder in 305 ml of ethanol. 64.9 (0.192 mol) of 4-chloro-3-(4-chloro-3-nitrophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole were added a little at a time to this mixture at 70-75° C. After 1 hour, 0.5 l of ethyl acetate was added and the solution was then filtered over a silica gel bed and subsequently concentrated. The residue was taken up in ethyl acetate. The ethyl acetate phase was washed with water, saturated sodium hydrogen carbonate solution and saturated sodium chloride solution, then dried over magnesium sulfate and finally concentrated. Yield: 56.4 g.

후처리

  1. filtrationthe solution was then filtered over a silica gel bed
  2. concentrationsubsequently concentrated
  3. washThe ethyl acetate phase was washed with water, saturated sodium hydrogen carbonate solution and saturated sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. concentrationfinally concentrated

출처 및 근거

ORD 기록
ord-94125d501f0f4b95bfd42abada888a3c
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05928999

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