Sodium Iodide → HCID 19018990、化合物

HRID 1110287ノート

反応式

HRID 1110287 の反応式
[CH3:1][O:2][C:3](=[O:37])[CH2:4][N:5]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[C:6]1[CH:11]=[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:9]=[C:8]([OH:31])[CH:7]=1.Br[CH2:39][CH2:40][CH2:41][O:42][C:43]1[CH:44]=[C:45]([Br:49])[CH:46]=[CH:47][CH:48]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CC(C)=O.CN(C=O)C>[CH3:1][O:2][C:3](=[O:37])[CH2:4][N:5]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[C:6]1[CH:11]=[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:9]=[C:8]([O:31][CH2:39][CH2:40][CH2:41][O:42][C:43]2[CH:48]=[CH:47][CH:46]=[C:45]([Br:49])[CH:44]=2)[CH:7]=1

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 19388979N-(2-methoxy-2-oxoethyl)-N-[3-hydroxy-5-(octadecyloxy)phenyl]glycine methyl esterHCID 193891331-Bromo-3-(3-bromopropoxy)benzene

生成物 1

HCID 19018990HCID 19018990、化合物収率 70%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1.0 g (1.92 mol) of N-(2-methoxy-2-oxoethyl)-N-[3-hydroxy-5-(octadecyloxy)phenyl]glycine methyl ester, 0.59 g (2.01 mmol) of 3-(3-bromopropoxy)bromobenzene, 0.53 g (3.83 mmol) of potassium carbonate and 0.29 g (1.92 mmol) of sodium iodide in 30 ml of acetone and 6 ml of DMF was stirred at reflux under argon for 65 hours. The solvents were removed at reduced pressure and the residue was treated with methylene chloride and filtered. The filtrate was concentrated and crystallized from methylene chloride-methanol to give 0.99 g (70%, mp 48°-50°) of N-(2-methoxy-2-oxoethyl)-N-[3-[3-(3-bromophenoxy)propoxy]-5-(octadecyloxy)phenyl]glycine methyl ester.

後処理

  1. temperatureat reflux under argon for 65 hours
  2. customThe solvents were removed at reduced pressure
  3. additionthe residue was treated with methylene chloride
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. customcrystallized from methylene chloride-methanol

出典と根拠

ORDレコード
ord-4b3c947dd98d442a9e857ad2f0bc3abd
出典データセット
uspto-grants-1994_06
特許番号
US05324747

反応ノート

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