Hydrochloric Acid → 4-[4-[8-(1,2,4-Triazol-1-yl)octyloxy]phenyl]benzoic acid

HRID 1872372노트

반응식

HRID 1872372 반응식
[H-].[Na+].[NH:3]1[CH:7]=[N:6][CH:5]=[N:4]1.Br[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:32]=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[CH:26][CH:25]=2)=[CH:20][CH:19]=1.Cl>CN(C)C=O.C(OCC)(=O)C.O>[N:3]1([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][C:18]2[CH:23]=[CH:22][C:21]([C:24]3[CH:25]=[CH:26][C:27]([C:28]([OH:30])=[O:29])=[CH:31][CH:32]=3)=[CH:20][CH:19]=2)[CH:7]=[N:6][CH:5]=[N:4]1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 211822604-[4-(8-Bromooctyloxy)phenyl]benzoic acid

생성물 1

HCID 211825254-[4-[8-(1,2,4-Triazol-1-yl)octyloxy]phenyl]benzoic acid수율 83.4%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

To a suspension of sodium hydride (60% suspension in mineral oil) (0.296 g) in N,N-dimethylformamide (14 ml) was added 1,2,4-triazole (0.511 g) and 4-[4-(8-bromooctyloxy)phenyl]benzoic acid (1 g), and was stirred for 5 hours at 120° C. The reaction mixture was added to a mixture of water and ethyl acetate, and adjusted to pH 2.5 with conc. hydrochloric acid. The organic layer was taken and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give 4-[4-[8-(1,2,4-Triazol-1-yl)octyloxy]phenyl]benzoic acid (0.81 g).

후처리

  1. dry with materialdried over magnesium sulfate
  2. filtrationThe magnesium sulfate was filtered off
  3. customthe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-329ceb64a1444dcca2fe65f243827d29
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107458

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