Triethylamine → HCID 178505620、化合物

HRID 1875437ノート

反応式

HRID 1875437 の反応式
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

参加物

6

反応物 2

HCID 8471TriethylamineHCID 178505619HCID 178505619、化合物

生成物 1

HCID 178505620HCID 178505620、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fc86dcb1e9fe489282a5ba655da449ce
出典データセット
uspto-grants-2012_11
特許番号
US08309551B2

反応ノート

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