Triethylamine → HCID 131737089、化合物

HRID 60383ノート

反応式

HRID 60383 の反応式
[Br:1][C:2]1[O:6][C:5]([CH:7]=[CH:8][C:9]([OH:11])=O)=[CH:4][CH:3]=1.C(N(CC)CC)C.ClC(OCC)=O.[N-:25]=[N+:26]=[N-:27].[Na+]>C(#N)C>[Br:1][C:2]1[O:6][C:5]([CH:7]=[CH:8][C:9]([N:25]=[N+:26]=[N-:27])=[O:11])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 33557Sodium AzideHCID 9460883-(5-Bromofuran-2-yl)prop-2-enoic acid

生成物 1

HCID 131737089HCID 131737089、化合物収率 44.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 3-(5-bromo-2-furyl)acrylic acid (41.5 g) in acetonitrile (200 mL) were added triethylamine (23.0 g) and ethyl chloroformate (26.1 g). The mixture was stirred at room temperature for 30 min. To the obtained mixture was added a saturated aqueous solution of sodium azide (18.7 g) at 0° C. and the mixture was stirred at room temperature for 5 hr. The reaction mixture was filtered, and the obtained solid was washed with water. The solid was recrystallized from dichloromethane to give the title compound (20.7 g) as white solid.

後処理

  1. stirringthe mixture was stirred at room temperature for 5 hr
  2. filtrationThe reaction mixture was filtered
  3. washthe obtained solid was washed with water
  4. customThe solid was recrystallized from dichloromethane

出典と根拠

ORDレコード
ord-f311bd1396044febb1d35e93ccc5e430
出典データセット
uspto-grants-2016_09
特許番号
US09440987B2

反応ノート

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