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Acetic Acid → (5-Bromo-2-iodo-benzyl)-ethyl-amine

HRID 1625664
ノート
印刷プレビュー

反応式

HRID 1625664 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:10])=[C:6]([CH:9]=1)[CH:7]=O.[CH2:11]([NH2:13])[CH3:12].C(O)(=O)C.C([BH3-])#N.[Na+]>CO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:10])=[C:6]([CH:9]=1)[CH2:7][NH:13][CH2:11][CH3:12]
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 176Acetic AcidHCID 6341EthylamineHCID 5003444Sodium cyanoborohydrideHCID 219738615-Bromo-2-iodobenzaldehyde

生成物 1

HCID 58148919(5-Bromo-2-iodo-benzyl)-ethyl-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 5-bromo-2-iodo-benzaldehyde (5.0 g, 16.1 mmol) in methanol (20 mL) was added ethylamine (2M in methanol; 16 mL, 24.0 mmol), followed by acetic acid (1.0 mL, 17.8 mmol), and the mixture was stirred at room temperature for 30 minutes. Sodium cyanoborohydride (2.0 g, 31.8 mmol) was then added over 5 minutes, and the reaction was stirred at room temperature over the weekend. The mixture was concentrated and partitioned between ethyl acetate and saturated aqueous sodium bicarbonate. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography (0-5% methanol in dichloromethane) to give the title compound.

後処理

  1. stirringthe reaction was stirred at room temperature over the weekend
  2. concentrationThe mixture was concentrated
  3. custompartitioned between ethyl acetate and saturated aqueous sodium bicarbonate
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. dry with materialthe combined organic layers were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by silica gel chromatography (0-5% methanol in dichloromethane)

出典と根拠

ORDレコード
ord-096e142eb4c94005bdc8aaae818bb679
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785393B2

反応ノート

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