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

HRID 1872372ノート

反応式

HRID 1872372 の反応式
[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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-329ceb64a1444dcca2fe65f243827d29
出典データセット
uspto-grants-2000_08
特許番号
US06107458

反応ノート

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