Hydrochloric Acid → HCID 23004093、化合物

HRID 1460241

反応式

HRID 1460241 の反応式
[C:1]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:20]>[Pd].C(O)(=O)C.CO.C(#N)C>[ClH:20].[C:1]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 772524-Benzhydrylpyridine

生成物 1

HCID 23004093HCID 23004093、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 21959252Acetonitrile methanol溶媒

実験手順

A mixture of 62.69 g (0.256 mole) of 4-(diphenylmethyl)pyridine and 6.4 g of 10% palladium on carbon (0.006 mole) in 300 ml of glacial acetic acid and under an atmosphere of hydrogen (44 psi) was shaken on a Parr apparatus at 85° for 4 days. The reaction mixture was filtered, and the solvent was removed in vacuo from the filtate. The residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give a solid. This was dissolved in a mixture of methanol-acetonitrile, and excess ethereal hydrogen chloride was added. A precipitate was collected to give 59.13 g (80.3%) of slightly impure title compound as a white, crystalline solid, mp 273°-274° C. Part of this was recrystallized from methanol-ether to give an analytically pure sample, mp 275.5°-277° C.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe solvent was removed in vacuo from the filtate
  3. customThe residue was partitioned between methylene chloride and dilute sodium hydroxide
  4. dry with materialThe methylene chloride solution was dried over magnesium sulfate
  5. customthe solvent was removed in vacuo
  6. customto give a solid
  7. additionwas added
  8. customA precipitate was collected

出典と根拠

ORDレコード
ord-84edd8f45d46465aaeb9c9f648310f83
出典データセット
uspto-grants-1991_12
特許番号
US05070087

関連ノート

読み込み中…