Sulfuric Acid → HCID 53936879, 화합물

HRID 845494노트

반응식

HRID 845494 반응식
[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]

참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 517045Sodium AcetateHCID 56994825HCID 56994825, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 53936879HCID 53936879, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매2회HCID 23948Rhodium촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f17a93c4863749e7a6f3b00ddea050a1
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758585

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