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Hydrochloric Acid → HCID 14722388、化合物

HRID 1031718
ノート
印刷プレビュー

反応式

HRID 1031718 の反応式
[CH3:1][S:2]([NH:5][C:6]1[C:24]([O:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:23][C:9]2[C:10](=[O:22])[C:11]([N:14]([CH:20]=[O:21])[CH2:15][C:16]([O:18]C)=[O:17])=[CH:12][O:13][C:8]=2[CH:7]=1)(=[O:4])=[O:3].Cl>[OH-].[Na+]>[CH3:1][S:2]([NH:5][C:6]1[C:24]([O:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:23][C:9]2[C:10](=[O:22])[C:11]([N:14]([CH2:15][C:16]([OH:18])=[O:17])[CH:20]=[O:21])=[CH:12][O:13][C:8]=2[CH:7]=1)(=[O:3])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 14722348HCID 14722348、化合物

生成物 1

HCID 14722388HCID 14722388、化合物収率 82.6%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

In 45 ml of a 1N aqueous sodium hydroxide solution was dissolved 4.46 g of 7-methylsulfonylamino- 3-(N-formyl-N-methoxycarbonylmethylamino)-6-phenoxy-4H-1-benzopyran-4-one. The solution was stirred for 1.5 hours at 25°-30° C. The solution was then adjusted to pH 3 with 4N hydrochloric acid and extracted with two 50-ml portions of ethyl acetate. The extracts (the organic layers) were combined, 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 mixed with diethyl ether. The resulting crystal was collected by filtration to obtain 3.57 g (yield: 82.6%) of 7-methylsulfonylamino-3-(N-carboxymethyl-N-formylamino)-6-phenoxy-4H-1-benzopyran-4-one having a melting point of 98°-100° C.

後処理

  1. extractionextracted with two 50-ml portions of ethyl acetate
  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. additionThe residue was mixed with diethyl ether
  6. filtrationThe resulting crystal was collected by filtration

出典と根拠

ORDレコード
ord-79e522e975d4441a8328444c98cb8352
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

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