Sodium Hydroxide → HCID 57285652、化合物

HRID 648660ノート

反応式

HRID 648660 の反応式
[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:17]([C:29]([NH2:31])=[O:30])[C:18]2[CH:28]=[CH:27][C:21]([C:22](OCC)=[O:23])=[CH:20][CH:19]=2)[CH2:14][CH2:15][CH3:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O1CCCC1>[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:17]([C:29]([NH2:31])=[O:30])[C:18]2[CH:19]=[CH:20][C:21]([CH2:22][OH:23])=[CH:27][CH:28]=2)[CH2:14][CH2:15][CH3:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 20145118HCID 20145118、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 57285652HCID 57285652、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 5.0 gm (11.83 m mol) of ethyl 4-[(1-(2-piperidino-phenyl)-1-butyl)-aminocarbonylmethyl]-benzoate in 75 ml of absolute tetrahydrofuran was added dropwise, at an internal temperature of 0° C., to a stirred suspension of 0.68 gm (17.95 m mol) of lithium aluminium hydride in 25 ml of absolute tetrahydrofuran. The mixture was stirred for 20 hours at ambient temperature and then cooled to 0° C., and 4N sodium hydroxide solution was slowly added dropwise thereto until a filterable precipitate formed. The mixture was filtered, and the precipitate was decocted several times with ether. The combined organic solutions were concentrated by evaporation in vacuo. The evaporation residue was distributed between water and ether. The ether phase was dried, filtered, and concentrated by evaporation in vacuo. The evaporation residue was purified by column chromatography on silica gel [toluene/acetone (5:1)].

後処理

  1. temperaturecooled to 0° C.
  2. customuntil a filterable precipitate formed
  3. filtrationThe mixture was filtered
  4. concentrationThe combined organic solutions were concentrated by evaporation in vacuo
  5. dry with materialThe ether phase was dried
  6. filtrationfiltered
  7. concentrationconcentrated by evaporation in vacuo
  8. customThe evaporation residue was purified by column chromatography on silica gel [toluene/acetone (5:1)]

出典と根拠

ORDレコード
ord-d4e62fc588d44899a207ba65363bfa9e
出典データセット
uspto-grants-1988_04
特許番号
US04735959

反応ノート

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