Triethylamine → HCID 58097361、化合物

HRID 2067830ノート

反応式

HRID 2067830 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([O:11][CH3:12])[C:5]([NH2:10])=[C:6]([O:8][CH3:9])[CH:7]=1.C(N(CC)CC)C.[C:20]([CH2:24][C:25](Cl)=[O:26])([CH3:23])([CH3:22])[CH3:21]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([O:11][CH3:12])[C:5]([NH:10][C:25](=[O:26])[CH2:24][C:20]([CH3:23])([CH3:22])[CH3:21])=[C:6]([O:8][CH3:9])[CH:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 815143,3-Dimethylbutanoyl chlorideHCID 3294234-Bromo-2,6-dimethoxyaniline

生成物 1

HCID 58097361HCID 58097361、化合物収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of the crude 5-bromo-1,3-dimethoxy-2-amino-benzene from above and triethylamine (1.5 g, 15 mmol) in anhydrous dichloromethane (50 mL) was added dropwise tert-butyl acetyl chloride (1.6 g, 12 mmol) with stirring at room temperature. The reaction mixture was stirred for 3 hours at room temperature. Then the reaction mixture was diluted with dichloromethane, washed with water, dried over anhydrous sodium sulfate, and evaporated to dryness under reduced pressure. The residue was purified by silica gel column (ISCO, hexane/EtOAc, 0-40%, 40 min) to give a white solid (3.0 g, 91%). 1H-NMR (DMSO-d6, 400 MHz): δ 8.69 (brs, 1H, exchangeable with D2O), 6.87 (s, 2H), 3.73 (s, 6H), 2.11 (s, 2H), 1.02 (s, 9H).

後処理

  1. stirringThe reaction mixture was stirred for 3 hours at room temperature
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated to dryness under reduced pressure
  5. customThe residue was purified by silica gel column (ISCO, hexane/EtOAc, 0-40%, 40 min)

出典と根拠

ORDレコード
ord-f2d8b3a07dfc439f9eeae9f0ea3b0e4d
出典データセット
uspto-grants-2012_10
特許番号
US08293911B2

反応ノート

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