Sodium Iodide → HCID 19018990, 화합물

HRID 1757843노트

반응식

HRID 1757843 반응식
[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

참가 물질

7

반응물 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

생성물 1

HCID 19018990HCID 19018990, 화합물수율 70.2%

시약·촉매·용매 2

HCID 180Acetone용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1.0 g (1.92 mmol) 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 wasconcentrated and crystallized from methylene chloride-methanol to give 0.99g (70%, mp 48°-50°) of N-(2-methoxy-2-oxoethyl)-N-[3-[3-(3-bromophenoxy) propoxy]-5-(octadecyloxy)phenyl]glycine methyl ester.

후처리

  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. customcrystallized from methylene chloride-methanol

출처 및 근거

ORD 기록
ord-66f035c8b545439db8398d0d0f4a0ecb
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05446189

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