Sodium Hydroxide → HCID 23695520, 화합물

HRID 2232626노트

반응식

HRID 2232626 반응식
C[O:2][C:3]([C:5]1([CH:8]([F:21])[CH2:9][CH2:10][CH2:11][CH2:12][O:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH2:7][O:6]1)=[O:4].[OH-].[Na+:23]>C(O)C.O>[Na+:23].[Cl:20][C:17]1[CH:16]=[CH:15][C:14]([O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH:8]([C:5]2([C:3]([O-:4])=[O:2])[CH2:7][O:6]2)[F:21])=[CH:19][CH:18]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 54007397HCID 54007397, 화합물

생성물 1

HCID 23695520HCID 23695520, 화합물수율 86.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 2-[5-(4-chlorophenoxy)-1-fluoropentyl]-2-oxiranecarboxylic acid methyl ester (2.53 g, 8 mmol) of Example 2 in 25 ml of absolute ethanol is treated with a solution of 320 mg (8 mmol) of sodium hydroxide in 12 ml of water. The mixture is maintained with stirring at room temperature for 2 hours and then is rotoevaporated. The obtained solid is triturated three times with ethyl ether, the solvent is removed by rotoevaporation and the solid is dried at high vacuum over phosphorus pentoxide to give 2.25 g (86.6%) of the title compound: m.p. 159°-175° C.; IR (KBr) 1630, 1608, 1490 and 1242 cm-1 ; NMR (d6 -DMSO) δ1.54 (2H, m), 1.73 (4H, m), 2.65 (1H, m), 2.73 (1H, d, J=6 Hz), 3.98 (2H, t, J=6 Hz), 5.22 (1H, ddd, JHF =48, 10, 3 Hz), 7.00 (2H, d, J=9 Hz) and 7.36 (2H, d, J=9 Hz).

후처리

  1. temperatureThe mixture is maintained
  2. customThe obtained solid is triturated three times with ethyl ether
  3. customthe solvent is removed by rotoevaporation
  4. dry with materialthe solid is dried at high vacuum over phosphorus pentoxide

출처 및 근거

ORD 기록
ord-81cf0ac80f9c45cc9ac017fe1808fb0b
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04788304

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