N-{4-[4-(2-Hydroxyethyloxy)phenyl]butyl}phthalimide → HCID 11537093、化合物

HRID 217926ノート

反応式

HRID 217926 の反応式
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][CH2:13][CH2:14][N:15]2C(=O)C3=CC=CC=C3C2=O)=[CH:7][CH:6]=1>CN.CO>[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][CH2:13][CH2:14][NH2:15])=[CH:7][CH:6]=1

参加物

4

反応物 1

HCID 22566183N-{4-[4-(2-Hydroxyethyloxy)phenyl]butyl}phthalimide

生成物 1

HCID 11537093HCID 11537093、化合物収率 35%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6329Methylamine溶媒

実験手順

The crude protected amine 114 (1.2 g, 35 mmol) was dissolved in 40 mL of a 2 N solution of methyl amine in dry methanol and the reaction mixture was stirred overnight at room temperature. After this time the solvent was removed under reduced pressure and the residue was purified by flash chromatography (silica gel, 5:1:0.1 chloroform/methanol/concentrated ammonium hydroxide) to give free amine 115 (0.25 g, 35%) as a clear oil. 1H NMR (300 MHz, DMSO-d6) δ 1.58 (m, 4H), 2.55 (m, 2H), 2.73 (m, 2H), 3.83 (m, 2H), 3.97 (m, 2H), 6.83 (d, 2H), 7.07 (d, 2H), 7.82 (s, 1H).

後処理

  1. customAfter this time the solvent was removed under reduced pressure
  2. customthe residue was purified by flash chromatography (silica gel, 5:1:0.1 chloroform/methanol/concentrated ammonium hydroxide)

出典と根拠

ORDレコード
ord-4fb156ffd7664eb4a412aaa4cef6e4b0
出典データセット
uspto-grants-2012_06
特許番号
US08198286B2

反応ノート

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