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Dichloromethane → HCID 15580690, 화합물

HRID 543816
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HRID 543816 반응식
[F:1][C:2]([F:24])([F:23])[C:3]([NH:5][C:6]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14](C(=O)C(F)(F)F)=[CH:13][CH:12]=2)[N:7]=1)=[O:4].ClCCl.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C(N(CC)CC)C>[F:24][C:2]([F:1])([F:23])[C:3]([NH:5][C:6]1[CH2:10][CH2:9][N:8]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:7]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 9845Trifluoroacetic anhydrideHCID 15580703HCID 15580703, 화합물

생성물 1

HCID 15580690HCID 15580690, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A mixture of 5.0 g. of 3-amino-1-phenyl-2-pyrazoline (prepared as described in Example 8), 200 ml. of dichloromethane, 5.0 ml. of triethylamine and 7.0 ml. of trifluoroacetic anhydride is allowed to remain at room temperature for 30 minutes. The mixture is evaporated to dryness in vacuo, then water is added to separate a semi-solid. The solid is dissolved in dichloromethane. The solution is dried over anhydrous sodium sulfate, columnized and recrystallized as for Example 14 (B) to give 3.0 g. of the desired product as yellow-orange prisms, m.p. 163°-165° C.

후처리

  1. additionA mixture of 5.0 g
  2. customThe mixture is evaporated to dryness in vacuo
  3. additionwater is added
  4. customto separate a semi-solid
  5. dissolutionThe solid is dissolved in dichloromethane
  6. dry with materialThe solution is dried over anhydrous sodium sulfate
  7. customto give 3.0 g

출처 및 근거

ORD 기록
ord-5d4db7243ba04afeb452c561b33da281
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04447442

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