Triethylamine → HCID 178505620, 화합물

HRID 1875437노트

반응식

HRID 1875437 반응식
Cl[C:2]1[CH:3]=[C:4]2[NH:10][N:9]=[C:8]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[F:18])[C:5]2=[N:6][CH:7]=1.C(N(CC)CC)C>C(O)C.C1COCC1.[Pd]>[F:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[CH2:11][C:8]1[C:5]2=[N:6][CH:7]=[CH:2][CH:3]=[C:4]2[NH:10][N:9]=1

참가 물질

6

반응물 2

HCID 8471TriethylamineHCID 178505619HCID 178505619, 화합물

생성물 1

HCID 178505620HCID 178505620, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

411 mg (1.57 mmol) of 6-chloro-3-(2-fluorobenzyl)-1H-pyrazolo[4,3-b]pyridine from example 3A are dissolved in a mixture of 4 ml of ethanol and 4 ml of THF, and, after addition of 159 mg (1.57 mmol) of triethylamine and 140 mg of 10% palladium on carbon, the mixture is hydrogenated under a hydrogen atmosphere at atmospheric pressure for 2 h. It is then filtered to remove the catalyst, concentrated in vacuo and taken up in water. The mixture is extracted with dichloromethane, and the organic phase is dried over sodium sulfate. Concentration results in 334 mg (94% of theory) of the title compound as white crystals.

후처리

  1. filtrationIt is then filtered
  2. customto remove the catalyst
  3. concentrationconcentrated in vacuo
  4. extractionThe mixture is extracted with dichloromethane
  5. dry with materialthe organic phase is dried over sodium sulfate
  6. concentrationConcentration

출처 및 근거

ORD 기록
ord-fc86dcb1e9fe489282a5ba655da449ce
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309551B2

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