1-Iodopropane → N-Propyl-N-[2-[4-(4,4,4-trifluoro-3,3-dimethoxybut-1-yl)phenoxy]ethyl]dodecylamine

HRID 1700915ノート

反応式

HRID 1700915 の反応式
[CH3:1][O:2][C:3]([O:32][CH3:33])([C:28]([F:31])([F:30])[F:29])[CH2:4][CH2:5][C:6]1[CH:27]=[CH:26][C:9]([O:10][CH2:11][CH2:12][NH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])=[CH:8][CH:7]=1.[CH:34](N(C(C)C)CC)([CH3:36])[CH3:35].ICCC>C(O)(C)C.C(OCC)(=O)C>[CH2:35]([N:13]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:12][CH2:11][O:10][C:9]1[CH:8]=[CH:7][C:6]([CH2:5][CH2:4][C:3]([O:2][CH3:1])([O:32][CH3:33])[C:28]([F:30])([F:31])[F:29])=[CH:27][CH:26]=1)[CH2:34][CH3:36]

参加物

6

反応物 3

HCID 336431-IodopropaneHCID 81531DiisopropylethylamineHCID 18319017N-[2-[4-(3,3-Dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]dodecylamine

生成物 1

HCID 18319117N-Propyl-N-[2-[4-(4,4,4-trifluoro-3,3-dimethoxybut-1-yl)phenoxy]ethyl]dodecylamine収率 96.8%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of N-[2-[4-(3,3-dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]dodecylamine (500 mg, 1.05 mmol), diisopropyl ethylamine (0.35 ml, 2.1 mmol) and 1-iodopropane (0.26 ml, 2.66 mmol) in isopropanol was heated to reflux for 21 h. After cooling to r.t., the mixture was diluted with ethyl acetate and filtered. The filtrate was concentrated in vacuo, and the residue was chromatographed on silica gel (dichloromethane/methanol 98:2 to 95:5) to afford the title compound (0.526 g, 73%) as a colorless oil.

後処理

  1. temperatureto reflux for 21 h
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in vacuo
  4. customthe residue was chromatographed on silica gel (dichloromethane/methanol 98:2 to 95:5)

出典と根拠

ORDレコード
ord-56f84f7b498443a397c23a7963392823
出典データセット
uspto-grants-2002_02
特許番号
US06350892B1

反応ノート

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