Hydrochloric Acid → HCID 86651355, 화합물

HRID 39496

반응식

HRID 39496 반응식
[Cl:1][CH:2]([CH2:6][OH:7])[C:3]([OH:5])=[O:4].[F:8][C:9]([F:35])([C:13]([F:34])([F:33])[C:14]([F:32])([F:31])[C:15]([F:30])([F:29])[C:16]([F:28])([F:27])[C:17]([F:26])([F:25])[C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20])[CH2:10][CH2:11]O.Cl>C(OCC)C>[F:8][C:9]([F:35])([C:13]([F:33])([F:34])[C:14]([F:31])([F:32])[C:15]([F:29])([F:30])[C:16]([F:27])([F:28])[C:17]([F:25])([F:26])[C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20])[CH2:10][CH2:11][O:4][C:3](=[O:5])[CH:2]([Cl:1])[CH2:6][OH:7]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 696191,1,2,2-Tetrahydroperfluoro-1-decanolHCID 5649512-Chloro-3-hydroxypropionic acid

생성물 1

HCID 86651355HCID 86651355, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
65 °C

실험 절차

In a 50 mL RB with a condenser, 2-chloro-3-hydroxypropionic acid (6.0 g, 0.05 mol) and 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-1-decanol (18.0 g, 0.04 mol) and a catalytic amount of hydrochloric acid were taken together and heated up to 65° C. for 36 h. Product was dissolved in 300 mL of ethyl ether and washed twice with 100 mL of dil. NaHCO3 aq. sol. and once with 100 mL of sat. aq. NaCl sol. and then dried over anhy. Na2SO4. Solution was filtered, solvent was removed by rotary evaporation and unreacted alcohol was sublimed off at 70° C. under vacuum. Yield=15.0 g (67%). 1H-NMR (CDCl3, 7.27 ppm): 2.54 (m, —CH2CF2). 3.05-3.35 (broad, —OH), 4.01 (m, —CH2OH), 4.42 (m, —CHCl), 4.52 (m, —CO2CH2CH2).

후처리

  1. washwashed twice with 100 mL of dil. NaHCO3 aq. sol. and once with 100 mL of sat. aq. NaCl sol.
  2. customdried over anhy
  3. filtrationSolution was filtered
  4. customsolvent was removed by rotary evaporation and unreacted alcohol
  5. customwas sublimed off at 70° C. under vacuum

출처 및 근거

ORD 기록
ord-677c3e9dab1e457ca7d7d2c5e85e43ce
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524942B2

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