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Dimethylformamide → HCID 58746070, 화합물

HRID 2110489
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HRID 2110489 반응식
[C:1]([O:5][C:6](=[O:18])[NH:7][C:8]1[C:9]2[N:10]([N:15]=[CH:16][CH:17]=2)[C:11](I)=[CH:12][CH:13]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:19][N:20](C=O)C>[C-]#N.[Zn+2].[C-]#N.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[C:1]([O:5][C:6](=[O:18])[NH:7][C:8]1[C:9]2[N:10]([N:15]=[CH:16][CH:17]=2)[C:11]([C:19]#[N:20])=[CH:12][CH:13]=1)([CH3:4])([CH3:3])[CH3:2]
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참가 물질

5

반응물 2

HCID 6228DimethylformamideHCID 58746000HCID 58746000, 화합물

생성물 1

HCID 58746070HCID 58746070, 화합물수율 93%

시약·촉매·용매 2

HCID 11186Zinc cyanide (Zn(CN)2)촉매HCID 11979704Tetrakis(triphenylphosphine)palladium촉매

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온도
80 °C

실험 절차

A mixture of (7-iodo-pyrazolo[1,5-a]pyridin-4-yl)-carbarnic acid tert-butyl ester (36 mg, 0.1 mmol), zinc cyanide (24 mg, 0.2 mmol), tetrakis(triphenylphosphine) palladium (0) (23 mg, 0.02 mmol), and anhydrous DMF (1 mL) was degassed with argon. Then, the mixture was stirred at 80° C. for 4.5 h, cooled to rt, mixed with EtOAc (6 mL), and filtered. The filtrate was concentrated under reduced pressure. Purification by silica gel flash chomatography eluting with EtOAc/heptane (gradient from 1:4 to 1:2 ratio) gave compound 777E (24 mg, 93%) as a white solid. HPLC: 93% at 3.64 min (retention time) (YMC S5 ODS-A column 4.6×50 mm eluting with 10-90% aqueous methanol over 4 mincontaining 0.2% phosphoric acid, 4 mL/min, monitoring at 220 nm). MS (ES): mn/z 259 [M+H]+.

후처리

  1. customwas degassed with argon
  2. temperaturecooled to rt
  3. additionmixed with EtOAc (6 mL)
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customPurification by silica gel flash chomatography
  7. washeluting with EtOAc/heptane (gradient from 1:4 to 1:2 ratio)

출처 및 근거

ORD 기록
ord-51a19d17e9634b61b82497e20caeeaaf
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07517904B2

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