Sulfuric Acid → HCID 53936879、化合物

HRID 845494ノート

反応式

HRID 845494 の反応式
[CH2:1]([CH:5]1[CH2:13][CH2:12][CH:11]2[CH:7]([C:8](=O)[C:9](=[O:14])[NH:10]2)[CH2:6]1)[CH2:2][CH2:3][CH3:4].[H][H].S(=O)(=O)(O)O.C([O-])(=O)C.[Na+]>C(O)(=O)C.[Pd].[Rh]>[CH2:1]([CH:5]1[CH2:13][CH2:12][CH:11]2[CH:7]([CH2:8][C:9](=[O:14])[NH:10]2)[CH2:6]1)[CH2:2][CH2:3][CH3:4]

参加物

8

反応物 4

HCID 1118Sulfuric AcidHCID 517045Sodium AcetateHCID 56994825HCID 56994825、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 53936879HCID 53936879、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒2 回HCID 23948Rhodium触媒HCID 176Acetic Acid溶媒

実験手順

For example, a solution of 5-n-butyl-octahydro-2,3-dioxo-1H-indole (III) (43.6 g, 0.214 mole) in acetic acid (250 ml) is treated with hydrogen gas in the presence of 20% Pd/C (2 g). Another 1 g of 20% Pd/C is added and concentrated sulfuric acid (1 ml) is added and the hydrogenation is continued. Ten percent Rh/C (2 g) is added and hydrogenation is continued. The suspension is filtered and sodium acetate (4.9 g, 0.06 mole) is added and the mixture is concentrated at reduced pressure The residue is recrystallized from cyclohexane with the use of activated carbon to yield pure 5-n-butyloctahydro-2-oxo-1H-indole (V) with a mp 109°-111° C.

後処理

  1. filtrationThe suspension is filtered
  2. concentrationthe mixture is concentrated at reduced pressure The residue
  3. customis recrystallized from cyclohexane with the use of activated carbon

出典と根拠

ORDレコード
ord-f17a93c4863749e7a6f3b00ddea050a1
出典データセット
uspto-grants-1988_07
特許番号
US04758585

反応ノート

読み込み中…