Potassium Carbonate → 2,3-Di-(2-methoxy ethoxy)propanol

HRID 865784노트

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HRID 865784 반응식
[OH:1][CH2:2][CH:3]1[CH2:20][O:19][CH2:18][CH2:17][O:16][CH2:15]COCCOC[CH2:8][O:7][CH2:6][CH2:5][O:4]1.C(OCC(OCCOC)COCCOC)(C)(C)C.F[B-](F)(F)F.[H+].C(OCC)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH3:8][O:7][CH2:6][CH2:5][O:4][CH:3]([CH2:20][O:19][CH2:18][CH2:17][O:16][CH3:15])[CH2:2][OH:1]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 36113931,4,7,10,13,16-Hexaoxacyclooctadecane-2-methanolHCID 16211330Borate(1-), tetrafluoro-, hydrogen, compd. with 1,1'-oxybis(ethane) (1:1:1)HCID 233746711-Tert-butyloxy-2,3-di-(2-methoxy ethoxy)propane

생성물 1

HCID 233746672,3-Di-(2-methoxy ethoxy)propanol

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Compound 29 was prepared by a method similar to that described by Montanari and Tundo20 for the synthesis of 2-(hydroxy methyl)-1,4,7,10,13,16-hexaoxacyclooctadecane. KBF4 complex, (2-(hydroxy methyl)-18-crown-6). To a solution of compound 23 (10.0 g, 0.038 mol.) in dichloromethane (100 ml) was added tetrafluoroboric acid-diethyl ether complex (54% in diethyl ether), (13.7 ml). The mixture was left stirring at room temperature for 20 minutes. The acid was neutralized with solid potassium carbonate, inorganic salts were filtered, the solvent was removed by rotary evaporation to give a pale yellow oil. The crude product was distilled under vacuum (bpt. 94°-95° C., 0.02 torr) to give a colorless liquid (18.75 g, 78%): 1H-NMR (CDCl3), d (ppm) 3.5-3.9 (m, 13H), 3.35-3.4 (s, 6H), 2.75-2.8 (s, 1H); 13C-NMR (CDCl3), d (ppm) 79.56, 72.07, 71.73, 71.16, 70.59, 69.35, 62.40, 58.83, 58.75.

후처리

  1. waitThe mixture was left
  2. filtrationwere filtered
  3. customthe solvent was removed by rotary evaporation
  4. customto give a pale yellow oil
  5. distillationThe crude product was distilled under vacuum (bpt. 94°-95° C., 0.02 torr)

출처 및 근거

ORD 기록
ord-9b03a1ab8e694ed5876b997afc9e5a94
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05567783

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