Formaldehyde → 3-(trifluoroacetyl)-1H-indole-1-ylmethanol

HRID 1983052ノート

反応式

HRID 1983052 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]([C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1)=[O:4].[CH2:16]=[O:17]>C(N(CC)CC)C.CC(C)=O>[F:15][C:2]([F:1])([F:14])[C:3]([C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]([CH2:16][OH:17])[CH:6]=1)=[O:4]

参加物

5

反応物 2

HCID 712FormaldehydeHCID 5891263-(Trifluoroacetyl)indole

生成物 1

HCID 231491933-(trifluoroacetyl)-1H-indole-1-ylmethanol収率 97.9%

試薬・触媒・溶媒 2

HCID 8471Triethylamine触媒HCID 180Acetone溶媒

反応条件

温度
130 °C

実験手順

The mixture of 4.80 g of 3-(trifluoroacetyl)-1H-indole, 1.35 g of paraformaldehyde and 0.10 g of triethylamine was stirred at 130° C. for 2 hours. After the reaction mixture was cooled to room temperature, acetone was added to the reaction mixture. The mixture was filtered, and then the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and hexane was added to the residue, as a result, a crystal was formed. The crystal was collected to obtain 5.36 g of 3-(trifluoroacetyl)-1H-indole-1-ylmethanol.

後処理

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionwas added to the residue, as a result
  5. customa crystal was formed
  6. customThe crystal was collected

出典と根拠

ORDレコード
ord-c0833845bd4d4bfc98159442bc2ddafb
出典データセット
uspto-grants-2009_06
特許番号
US07541374B2

反応ノート

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