Sulfate Ion → N-(2-((2-hydroxy-3-(4-(2-cyclobutylmethoxyethoxy)phenoxy)propyl)amino)ethyl)-4-morpholinecarboxamide

HRID 980162노트

반응식

HRID 980162 반응식
S([O-])([O-])(=O)=O.[NH2:6][CH2:7][CH2:8][NH:9][C:10]([N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1)=[O:11].[OH-].[Na+].[CH:20]1([CH2:24][O:25][CH2:26][CH2:27][O:28][C:29]2[CH:39]=[CH:38][C:32]([O:33][CH:34]3[O:37][CH:35]3[CH3:36])=[CH:31][CH:30]=2)[CH2:23][CH2:22][CH2:21]1>C(O)C>[OH:37][CH:35]([CH2:34][O:33][C:32]1[CH:38]=[CH:39][C:29]([O:28][CH2:27][CH2:26][O:25][CH2:24][CH:20]2[CH2:23][CH2:22][CH2:21]2)=[CH:30][CH:31]=1)[CH2:36][NH:6][CH2:7][CH2:8][NH:9][C:10]([N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1)=[O:11]

참가 물질

6

반응물 4

HCID 1117Sulfate IonHCID 14798Sodium HydroxideHCID 11041198N-(2-Aminoethyl)-4-morpholinecarboxamideHCID 867412074-(2-Cyclobutylmethoxyethoxy)phenoxy-1,2-epoxypropane

생성물 1

HCID 20222111N-(2-((2-hydroxy-3-(4-(2-cyclobutylmethoxyethoxy)phenoxy)propyl)amino)ethyl)-4-morpholinecarboxamide

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

12.0 g of the neutral sulphate of N-2-aminoethyl-4-morpholinecarboxamide and 2.16 g NaOH was refluxed in 100 ml of ethanol for 1 h. Thereafter 10 g of 3-(4-(2-cyclobutylmethoxyethoxy)phenoxy-1,2-epoxypropane in 50 ml of ethanol was added and the mixture refluxed for 20 h, filtered, and evaporated. The residue was dissolved in 175 ml of ethyl acetate and washed twice with water. Thereafter the title compound crystallized from the ethyl acetate phase. The crystals were filtered off and washed with ether. Yield 7.1 g. Melting point 91°-93° C. (base). The structure was determined using NMR-analysis.

후처리

  1. temperaturethe mixture refluxed for 20 h
  2. filtrationfiltered
  3. customevaporated
  4. dissolutionThe residue was dissolved in 175 ml of ethyl acetate
  5. washwashed twice with water
  6. customThereafter the title compound crystallized from the ethyl acetate phase
  7. filtrationThe crystals were filtered off
  8. washwashed with ether

출처 및 근거

ORD 기록
ord-5c5a26d1ff074d4784a66c18afa989e5
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636501

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