Acetic Acid → 1-Acetyl-5-carbomethoxy-7-chloro-4-methoxy-1,2-dihydroindole

HRID 2074002ノート

反応式

HRID 2074002 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[C:8]([O:18][CH3:19])[C:9]([C:14]([O:16][CH3:17])=[O:15])=[CH:10][C:11]=2[Cl:13])[CH:6]=[CH:5]1)(=[O:3])[CH3:2].C(O)(=O)C>[Pt].CO>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([O:18][CH3:19])[C:9]([C:14]([O:16][CH3:17])=[O:15])=[CH:10][C:11]=2[Cl:13])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 176Acetic AcidHCID 104931031-Acetyl-5-carbomethoxy-7-chloro-4-methoxyindole

生成物 1

HCID 105649501-Acetyl-5-carbomethoxy-7-chloro-4-methoxy-1,2-dihydroindole

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 887Methanol溶媒

実験手順

The mixture of the indole of step 8 above (0.9 g) and Pt-C (0.2 g), acetic acid and MeOH (100 ml) is stirred under H2 at 1 atm. pressure for 48 hours. The catalyst is filtered (celite), the filtered material is washed (MeOH) and the reaction mixture and methanol washings are evaporated. The residue is diluted with CH2Cl2, washed with saturated NaHCO3, dried (MgSO4) and evaporated affording a colorless, semicrystalline material which is determined to be the desired compound by NMR. M.P. 107°-109° C.

後処理

  1. filtrationThe catalyst is filtered (celite)
  2. washthe filtered material is washed (MeOH)
  3. customthe reaction mixture and methanol washings are evaporated
  4. additionThe residue is diluted with CH2Cl2
  5. washwashed with saturated NaHCO3
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. customaffording a colorless, semicrystalline material which

出典と根拠

ORDレコード
ord-be1d126f7a2a4da2bef77007ed389b1e
出典データセット
uspto-grants-1990_04
特許番号
US04920219

反応ノート

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