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Formic Acid → HCID 15580719, 화합물

HRID 1702655
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HRID 1702655 반응식
FC(F)(F)[C:3]([NH:5][C:6]1[CH2:10][CH:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:8]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)[N:7]=1)=[O:4].C(O)=O.ClC1C=C(N2CC(C)C(NC=O)=N2)C=CC=1Cl>O>[F:23][C:20]1[CH:19]=[CH:18][C:17]([N:8]2[CH:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:10][C:6]([NH:5][CH:3]=[O:4])=[N:7]2)=[CH:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 15580700HCID 15580700, 화합물HCID 15580721HCID 15580721, 화합물

생성물 1

HCID 15580719HCID 15580719, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 5.0 g. of 3-amino-1-(p-fluorophenyl)-5-phenyl-2-pyrazoline (prepared as described in Example 43) and 85.0 ml. of a mixture of formic acid and acetic anhydride (Example 15) is allowed to remain at room temperature for 2 hours. The solvent is evaporated in vacuo to give an oil. Water is added to separate a solid. The solid is dissolved in dichloromethane and is columnized and recrystallized twice as described in Example 26 (A) to give 3.55 g. of the desired product as colorless crystals, m.p. 158.5°-160.5° C.

후처리

  1. additionA mixture of 5.0 g
  2. customThe solvent is evaporated in vacuo
  3. customto give an oil
  4. customto separate a solid
  5. dissolutionThe solid is dissolved in dichloromethane
  6. customrecrystallized twice
  7. customto give 3.55 g

출처 및 근거

ORD 기록
ord-5e2e9a0b32ff411882fd7533e12c7707
출처 데이터셋
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04348527

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