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Methyl formate → HCID 19852111, 화합물

HRID 1607232
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인쇄 미리보기

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HRID 1607232 반응식
C(NC(C)C)(C)C.C([Li])CCC.[F:13][C:14]([F:39])([F:38])[O:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]([N:25]2[CH2:29][CH:28]([CH3:30])[C:27]([C:31]3[CH:36]=[CH:35][C:34]([Cl:37])=[CH:33][CH:32]=3)=[N:26]2)=[O:24])=[CH:18][CH:17]=1.[CH:40](OC)=[O:41]>O1CCCC1.CCCCCC.C(O)(=O)C>[F:39][C:14]([F:13])([F:38])[O:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]([N:25]2[CH2:29][C:28]([CH:40]=[O:41])([CH3:30])[C:27]([C:31]3[CH:36]=[CH:35][C:34]([Cl:37])=[CH:33][CH:32]=3)=[N:26]2)=[O:24])=[CH:18][CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 7865Methyl formateHCID 7912DiisopropylamineHCID 19852119HCID 19852119, 화합물HCID 178418339Butyllithium

생성물 1

HCID 19852111HCID 19852111, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid용매
HCID 8028
Tetrahydrofuran
용매
2회
HCID 8058Hexane용매

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온도
-20 °C

실험 절차

To 3.5 ml of diisopropylamine dissolved in 20 ml of tetrahydrofuran and cooled in a -20° C. bath was added 10.0 ml of a 2.5 molar solution n-butyllithium in hexane. After stirring for 5 minutes a solution of 4.0 g of N-(4-trifluoromethoxyphenyl)-3-(4-chlorophenyl)-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide in 10 ml of tetrahydrofuran was added and the resulting solution stirred for 15 minutes and then cooled to -78° C. To this solution was added 2.0 ml of methyl formate and, after 5 minutes, 2 ml of acetic acid was added. The reaction mixture was partitioned between diethyl ether and water and the organic layer was dried over anhydrous magnesium sulfate. The resulting solution was filtered, evaporated in vacuo to give 3.9 g of N-(4-trifluoromethoxyphenyl)-3-(4-chlorophenyl)-4-formyl-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide. NMR and IR data were consistent with the structure.

후처리

  1. additionwas added
  2. temperaturecooled to -78° C
  3. waitafter 5 minutes
  4. customThe reaction mixture was partitioned between diethyl ether and water
  5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationThe resulting solution was filtered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-882bb59e6ef34b348be5635b4728e2ea
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04863947

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