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Methanol → 2,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoic acid

HRID 659933
ノート
印刷プレビュー

反応式

HRID 659933 の反応式
CO.[Cl:3][C:4]1[C:14]([O:15][CH2:16][CH2:17][N:18]2[CH:22]=[N:21][N:20]=[N:19]2)=[C:13]([Cl:23])[CH:12]=[CH:11][C:5]=1[C:6]([O:8]CC)=[O:7].[OH-].[Na+]>O>[Cl:3][C:4]1[C:14]([O:15][CH2:16][CH2:17][N:18]2[CH:22]=[N:21][N:20]=[N:19]2)=[C:13]([Cl:23])[CH:12]=[CH:11][C:5]=1[C:6]([OH:8])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium Hydroxide2 回HCID 57437285ethyl 2,4-dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoate

生成物 1

HCID 574372702,4-Dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoic acid収率 85.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a methanol (15 ml) solution of ethyl 2,4-dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoate (0.88 g) were added sodium hydroxide (0.16 g) and water (5 ml), and the mixture was stirred at room temperature for 7 hours. After the addition of water (20 ml) and concentration at reduced pressure, an aqueous sodium hydroxide solution was added and the mixture was washed with ethyl acetate (50 ml). The aqueous layer was acidified with hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off to obtain the desired 2,4-dichloro-3-[2-(1H-tetrazol-1-yl)ethyloxy]-benzoic acid (0.69 g).

後処理

  1. washthe mixture was washed with ethyl acetate (50 ml)
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationEthyl acetate was distilled off

出典と根拠

ORDレコード
ord-104bb2c3b6624ea28e6352b3d5e9c5a9
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084398B2

反応ノート

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