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Benzyl Bromide → 1-(Benzyloxy)-3-bromo-5-iodobenzene

HRID 1189980
ノート
印刷プレビュー

反応式

HRID 1189980 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([I:8])[CH:7]=1.[CH2:10](Br)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C([O-])([O-])=O.[K+].[K+]>CN1C(=O)CCC1>[CH2:10]([O:9][C:4]1[CH:5]=[C:6]([I:8])[CH:7]=[C:2]([Br:1])[CH:3]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 226301823-Bromo-5-iodophenol

生成物 1

HCID 672965731-(Benzyloxy)-3-bromo-5-iodobenzene

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of 3-bromo-5-iodophenol (1.40 g, 4.68 mmol), benzyl bromide (0.89 g, 5.20 mmol) and anhydrous K2CO3 (1.44 g, 10.4 mmol) in anhydrous NMP (8 mL) was stirred under argon at +70° C. for 1 hour. The reaction mixture was partitioned between aqueous NH4Cl and hexanes. Aqueous layer was additionally extracted with hexanes and combined organic layers were washed with 1N NaOH, brine, dried over anhydrous MgSO4 and concentrated under reduced pressure to give 1-(benzyloxy)-3-bromo-5-iodobenzene as a colorless oil. Yield (2.14 g, 99%); 1H NMR (400 MHz, CDCl3) δ 7.45 (t, J=1.4 Hz, 1H), 7.32-7.40 (m, 5H), 7.26 (dd, J=1.4, 2.2 Hz, 1H), 7.09 (t, J=2.0 Hz, 1H), 5.00 (s, 2H).

後処理

  1. customThe reaction mixture was partitioned between aqueous NH4Cl and hexanes
  2. extractionAqueous layer was additionally extracted with hexanes
  3. washwere washed with 1N NaOH, brine
  4. dry with materialdried over anhydrous MgSO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e001cf20ac6e4a28aecdcb3844580aeb
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08674137B2

反応ノート

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