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Dichloromethane → HCID 89924168, 화합물

HRID 1505680
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HRID 1505680 반응식
I[C:2]1[CH:3]=[C:4]([C:8]2[N:13]=[CH:12][C:11]([C:14]3[CH:15]=[N:16][N:17]([CH:19]4[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:21][CH2:20]4)[CH:18]=3)=[CH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[C:32]([Si:34]([CH3:37])([CH3:36])[CH3:35])#[CH:33].C(Cl)Cl>C1COCC1.CN(C=O)C.CCOC(C)=O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].[Cu]I>[C:28]([O:27][C:25]([N:22]1[CH2:23][CH2:24][CH:19]([N:17]2[CH:18]=[C:14]([C:11]3[CH:10]=[N:9][C:8]([C:4]4[CH:5]=[CH:6][CH:7]=[C:2]([C:33]#[C:32][Si:34]([CH3:37])([CH3:36])[CH3:35])[CH:3]=4)=[N:13][CH:12]=3)[CH:15]=[N:16]2)[CH2:20][CH2:21]1)=[O:26])([CH3:31])([CH3:30])[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 3

HCID 6344DichloromethaneHCID 66111TrimethylsilylacetyleneHCID 89924119HCID 89924119, 화합물2회

생성물 1

HCID 89924168HCID 89924168, 화합물수율 39%

시약·촉매·용매 5

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매
HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of tert-butyl 4-{4-[2-(3-iodophenyl)pyrimidin-5-yl]-1H-pyrazol-1-yl}piperidine-1-carboxylate (intermediate 18, 315 mg; 0.59 mmol; 1.0 eq.), Ethynyl-trimethyl-silane (83 μl; 0.59 mmol; 1.0 eq.), (dppf)PdCl2.CH2Cl2 (26 mg; 0.04 mmol; 0.06 eq.), CuI (7 mg; 0.04 mmol; 0.06 eq.) and TEA (115 μl; 0.89 mmol; 1.5 eq.) in dry THF (3.6 mL) and dry DMF (1 mL) was heated in a sealed vial at 80° C. for 48 h. The reaction mixture was then diluted with EtOAc and washed with sat. NH4Cl and brine. Organic phase was dried over magnesium sulfate, filtered and concentrated. Purification by flash chromatography on silica (heptanes:EtOAC, gradient form 90:10 to 50:50) afforded the title compound as a beige solid (115 mg, 39%). 1H NMR (300 MHz, DMSO-d6) d 9.17 (s, 2H), 8.57 (s, 1H), 8.41-8.38 (m, 1H), 8.15 (s, 2H), 7.61-7.54 (m, 2H), 4.08-4.03 (m, 2H), 2.96 (m, 2H9, 2.08-2.05 (m, 2H), 1.83-1.77 (m, 2H), 1.43 (s, 9H), 0.26 (s, 9H). MS (ESI+): 502.5.

후처리

  1. washwashed with sat. NH4Cl and brine
  2. dry with materialOrganic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customPurification by flash chromatography on silica (heptanes:EtOAC, gradient form 90:10 to 50:50)

출처 및 근거

ORD 기록
ord-6cbe6fbc1a604dd29b0a4c2d99cfddfb
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216991B2

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