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Methanol → Methyl 2-amino-5-methoxy-4-phenylbenzoate

HRID 454505
ノート
印刷プレビュー

反応式

HRID 454505 の反応式
S(=O)(=O)(O)O.CO.[NH2:8][C:9]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:15]([O:24][CH3:25])=[CH:14][C:10]=1[C:11]([OH:13])=[O:12].[C:26](=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[NH2:8][C:9]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:15]([O:24][CH3:25])=[CH:14][C:10]=1[C:11]([O:13][CH3:26])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 669901042-Amino-5-methoxy-4-phenylbenzoic acid

生成物 1

HCID 66990992Methyl 2-amino-5-methoxy-4-phenylbenzoate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Under ice-cooling, concentrated sulfuric acid (1 mL) was added to a methanol (10 mL) suspension of the obtained 2-amino-5-methoxy-4-phenylbenzoic acid, followed by heating to reflux for 6 hours. The reaction mixture was cooled to room temperature and adjusted to a pH of 8.0 with a saturated aqueous solution of sodium bicarbonate, and then chloroform was added thereto. The organic layer was separated and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Hexane was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.24 g of methyl 2-amino-5-methoxy-4-phenylbenzoate as a brown solid.

後処理

  1. temperatureUnder ice-cooling
  2. temperatureby heating
  3. temperatureto reflux for 6 hours
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. additionHexane was added to the obtained residue
  8. filtrationthe solid substance was collected by filtration

出典と根拠

ORDレコード
ord-0da5db24d20d49aca92694c62330814b
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492582B2

反応ノート

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