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Dichloromethane → HCID 57423921, 화합물

HRID 2064081
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HRID 2064081 반응식
CC(C)([O-])C.[Na+].[F:7][CH:8]([F:34])[O:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]([NH:19][CH:20]2[CH2:25][CH2:24][N:23]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH2:22][CH2:21]2)=[O:18])=[C:12](I)[CH:11]=1.ClCCl>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[F:7][CH:8]([F:34])[O:9][C:10]1[CH:15]=[CH:14][C:13]2[NH:16][C:17](=[O:18])[N:19]([CH:20]3[CH2:25][CH2:24][N:23]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH2:22][CH2:21]3)[C:12]=2[CH:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6344DichloromethaneHCID 23676156Sodium t-butoxideHCID 59863024HCID 59863024, 화합물

생성물 1

HCID 57423921HCID 57423921, 화합물

시약·촉매·용매 3

HCID 635956Ferrocene-1,1'-bis-(diphenylphosphine)촉매
HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

A solution of tris(dibenzylideneacetone)dipalladium (0) (0.18 g), 1,1′-bis(diphenylphosphino)ferrocene (0.10 g), sodium tert-butoxide (0.6 g) in 1,4-dioxane (10 ml) was stirred under an atmosphere of argon for 10 minutes. 1,1-Dimethylethyl 4-{[({4-[(difluoromethyl)oxy]-2-iodophenyl}amino)carbonyl]amino}-1-piperidinecarboxylate (D52, 1.3 g) was added and the mixture was heated to 90° C. The mixture was stirred at this temperature overnight. The mixture was poured into dichloromethane which was washed with water and brine. The solvent was removed and the residue was chromatographed on silica gel eluted with ethyl acetate/hexane 0-50% to give the title compound as a off-white solid. (0.54 g).

후처리

  1. washwas washed with water and brine
  2. customThe solvent was removed
  3. customthe residue was chromatographed on silica gel
  4. washeluted with ethyl acetate/hexane 0-50%

출처 및 근거

ORD 기록
ord-a505bc2b45b1438391c4cb19371628c7
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288413B2

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