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Toluene → 5-Bromobenzofuran-2-carboxylic Acid Diethylamide

HRID 1860623
ノート
印刷プレビュー

反応式

HRID 1860623 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10](Cl)=[O:11])=[CH:7][C:6]=2[CH:13]=1.[CH2:14]([N:16](C(C)C)[CH:17](C)[CH3:18])[CH3:15].C1(C)C=CC=CC=1.C(NCC)C>O>[CH2:14]([N:16]([CH2:17][CH3:18])[C:10]([C:8]1[O:9][C:5]2[CH:4]=[CH:3][C:2]([Br:1])=[CH:13][C:6]=2[CH:7]=1)=[O:11])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1140TolueneHCID 8021DiethylamineHCID 81531DiisopropylethylamineHCID 27955345-Bromobenzo[b]furan-2-carbonyl chloride

生成物 1

HCID 99481065-Bromobenzofuran-2-carboxylic Acid Diethylamide収率 88%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.3 g. of 5-bromobenzofuran-2-carbonyl chloride, 1 mL [sic] of ethyldiisopropylamine and 30 mL [sic] of toluene are mixed and 0.62 ml of diethylamine is added to the brown-coloured solution with stirring. A precipitate is formed with a slightly exothermic reaction. After 5 minutes, the mixture was treated with 30 ml of completely deionized water and the phases were separated. The organic phase was washed with 1.) 20 ml of iN HCl 2.) 20 ml of iN NaOH 3.) 20 ml of water and then with 20 ml of saturated NaCl solution and then freed of solvent components in vacuo. After chromatography on silica gel the residual, yellowish oil forms in the eluent MtB ether/heptane 2:1 [sic]. Final weight: 1.3 g of colourless crystals [sic] (yield: 88%), m.p. 79-81°.

後処理

  1. customA precipitate is formed with a slightly exothermic reaction
  2. customthe phases were separated
  3. washThe organic phase was washed with 1

出典と根拠

ORDレコード
ord-e9a61a07ea404af9b3049a840a309c3b
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06531503B1

反応ノート

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