1,3-Dibromopropane → HCID 58097204、化合物

HRID 62153

反応式

HRID 62153 の反応式
[OH-].[K+].[Br:3][C:4]1[CH:5]=[CH:6][C:7]2[NH:8][C:9]3[C:14]([C:15]=2[CH:16]=1)=[CH:13][C:12]([Br:17])=[CH:11][CH:10]=3.[Br:18][CH2:19][CH2:20][CH2:21]Br>CN(C=O)C.CCOC(C)=O>[Br:17][C:12]1[CH:11]=[CH:10][C:9]2[N:8]([CH2:21][CH2:20][CH2:19][Br:18])[C:7]3[C:15]([C:14]=2[CH:13]=1)=[CH:16][C:4]([Br:3])=[CH:5][CH:6]=3

参加物

6

反応物 3

HCID 80011,3-DibromopropaneHCID 14797Potassium HydroxideHCID 2748743,6-Dibromocarbazole

生成物 1

HCID 58097204HCID 58097204、化合物収率 28.6%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

Crushed KOH (0.0673 g, 1.20 mmol, 1.2 equiv) was added to 3,6-dibromocarbazole (0.3250 g, 1.00 mmol) in 2 mL DMF solution and the mixture was stirred for 30 min. 1,3-dibromopropane (0.5047 g, 2.50 mmol, 2.5 equiv) in 3 mL DMF solution was added dropwise into the mixture and it was stirred at room temperature overnight. The crude reaction mixture was diluted with 30 mL EtOAc and washed with 1M HCl 2×10 mL and water 3×10 mL. The organic layer was dried over anhydrous Na2SO4 and evaporated to afford the crude product, which was subjected to silica gel chromatography using Hexanes/EtOAc to afford 0.1275 g colorless oil as product, yield 28.6%.

後処理

  1. stirringwas stirred at room temperature overnight
  2. customThe crude reaction mixture
  3. washwashed with 1M HCl 2×10 mL and water 3×10 mL
  4. dry with materialThe organic layer was dried over anhydrous Na2SO4
  5. customevaporated
  6. customto afford the crude product, which

出典と根拠

ORDレコード
ord-8148a197ba224f0199ad9a7179b4cc06
出典データセット
uspto-grants-2016_09
特許番号
US09446022B2

関連ノート

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