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Hydrochloric Acid → HCID 14722395、化合物

HRID 1031682
ノート
印刷プレビュー

反応式

HRID 1031682 の反応式
[C:1](OC(=O)C)(=[O:3])[CH3:2].[OH:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12].[C:35]([O-])(=O)[CH3:36].[Na+].Cl>O.C(OCC)(=O)C>[C:1]([N:23]([C:21]1[C:20]([O:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[CH:19][C:10]2[C:11](=[O:12])[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:35]([CH3:36])[O:8][C:9]=2[CH:22]=1)[S:24]([CH3:27])(=[O:26])=[O:25])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 10620577HCID 10620577、化合物

生成物 1

HCID 14722395HCID 14722395、化合物収率 55.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

2.55 ml of acetic anhydride was added to 850 mg of ethyl 2-(2-hydroxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate and 540 mg of sodium acetate. The mixture was stirred for 10 minutes at 110°-120° C. The reaction mixture was introduced into a mixture of 20 ml of ethyl acetate and 20 ml of water. The resulting mixture was adjusted to pH 2 with 2N hydrochloric acid. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: a 5 : 1 mixture of toluene and ethyl acetate) to obtain 550 mg (yield: 55.6%) of 7-(N-acetyl-N-methylsulfonylamino)-3-ethoxycarbonyl-2-methyl-6-phenoxy-4H-1-benzopyran-4-one.

後処理

  1. customThe organic layer was separated
  2. washwashed with water
  3. dry with materiala saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by a column chromatography (eluant
  6. additiona 5 : 1 mixture of toluene and ethyl acetate)

出典と根拠

ORDレコード
ord-a431ed6f23544814a75aebda73c6481c
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04954518

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート