1-Chloro-4-(chloromethyl)benzene → HCID 70565216、化合物

HRID 1427212ノート

反応式

HRID 1427212 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH2:11])[C:5]2[CH:6]=[CH:7][NH:8][C:9]=2[CH:10]=1.[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([CH2:17]Cl)=[CH:15][CH:14]=1.[OH-].[Na+]>>[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([CH2:17][N:8]2[C:9]3[CH:10]=[C:2]([F:1])[CH:3]=[C:4]([NH2:11])[C:5]=3[CH:6]=[CH:7]2)=[CH:15][CH:14]=1

参加物

4

反応物 3

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 14798Sodium HydroxideHCID 247280226-Fluoro-1H-indol-4-amine

生成物 1

HCID 70565216HCID 70565216、化合物

反応条件

温度
60 °C

実験手順

A mixture of 6-fluoro-1H-indol-4-amine (5 g, 0.033 mol), 4-chlorobenzyl chloride (5.55 g, 0.035 mol) and sodium hydroxide (1.32 g, 0.033 mol) was heated at 60° C. for 3 h. The solvent was evaporated and the residue was dissolved in EA (150 mL) and water (70 mL). The aqueous layer was extracted with EA and washed with brine (100 mL), dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel flash chromatography (PE:EA=8:1) to afford the title compound. LC/MS m/z=275.1 [M+H]+.

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was dissolved in EA (150 mL)
  3. extractionThe aqueous layer was extracted with EA
  4. washwashed with brine (100 mL)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by silica gel flash chromatography (PE:EA=8:1)

出典と根拠

ORDレコード
ord-d6803544e7cd4af88acfbb7b26573fd4
出典データセット
uspto-grants-2015_01
特許番号
US08933113B2

反応ノート

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