Water → HCID 9887502、化合物

HRID 985602ノート

反応式

HRID 985602 の反応式
I[CH2:2][C:3]1([CH3:19])[O:18][C:6]2=[C:7]([CH3:17])[C:8]3[CH2:9][C:10]([CH3:16])([CH3:15])[NH:11][C:12]=3[C:13]([CH3:14])=[C:5]2[CH2:4]1.[C:20]1([CH:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.[K].O>CN(C)C(=O)C>[CH3:19][C:3]1([CH2:2][N:29]2[CH2:30][CH2:31][CH:26]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:27][CH2:28]2)[O:18][C:6]2=[C:7]([CH3:17])[C:8]3[CH2:9][C:10]([CH3:16])([CH3:15])[NH:11][C:12]=3[C:13]([CH3:14])=[C:5]2[CH2:4]1

参加物

6

反応物 4

HCID 962WaterHCID 698734-PhenylpiperidineHCID 5462222PotassiumHCID 22506876HCID 22506876、化合物

生成物 1

HCID 9887502HCID 9887502、化合物収率 62%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
180 °C

実験手順

A suspension of 3,5,6,7-tetrahydro-2-(iodomethyl)-2,4,6,6,8-pentamethyl-2H-furo[2,3-f]indole (1.11 g, 2.99 mmol), 4-phenylpiperidine (723 mg, 4.48 mmol) and potassium carboante (826 mg, 5.98 mmol) in N,N-dimethylacetamide (6 ml) was stirred for 3 hours at 180° C. under nitrogen atmosphere. To the reaction mixture was added water, and extracted three times with ethyl acetate. The organic layers were combined, washed with water and saturated brine, dried over magnesium sulfate, treated with an active charcoal, filtered and then concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to obtain 744 mg of the title compound.

後処理

  1. extractionextracted three times with ethyl acetate
  2. washwashed with water and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. additiontreated with an active charcoal
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-4fcd8ed683b34a3b9da57c7b4432d5cf
出典データセット
uspto-grants-2005_03
特許番号
US06872718B1

反応ノート

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