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Hydrochloric Acid → 5-Amino-3-mercapto-4-phenoxybenzoic acid

HRID 1605512
ノート
印刷プレビュー

反応式

HRID 1605512 の反応式
[Na].[N+:2]([C:5]1[C:6]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[C:7]([S:14](O)=O)[CH:8]=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11])([O-])=O.Cl>C(O)C.[Zn]>[NH2:2][C:5]1[C:6]([O:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)=[C:7]([SH:14])[CH:8]=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11]
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 3

HCID 313Hydrochloric AcidHCID 5360545SodiumHCID 215201035-Nitro-4-phenoxy-3-sulfinobenzoic acid

生成物 1

HCID 215201075-Amino-3-mercapto-4-phenoxybenzoic acid

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

Zinc powder (38 g) is added to a warm solution (70° C) of the mono sodium salt of 5-nitro-4-phenoxy-3-sulfinobenzoic acid (10 g) in ethanol (190 ml), and while stirring 5 N hydrochloric acid (190 ml) is added dropwise. The reaction mixture is kept under nitrogen for an additional 2 hours at 70° C. After cooling and filtration, the ethanol is distilled off in vacuo. After standing in a refrigerator for 16 hours, the precipitated material is collected by filtration and washed with concentrated hydrochloric acid (15 ml). This material is then suspended in water (300 ml) and the pH adjusted to 2 by addition of 2 N sodium hydroxide. The obtained crude 5-amino-3-mercapto-4-phenoxybenzoic acid is collected and recrystallized from aqueous ethanol. The acid is obtained with a melting point of 199°-200° C.

後処理

  1. additionis added dropwise
  2. temperatureAfter cooling
  3. filtrationfiltration
  4. distillationthe ethanol is distilled off in vacuo
  5. waitAfter standing in a refrigerator for 16 hours
  6. filtrationthe precipitated material is collected by filtration
  7. washwashed with concentrated hydrochloric acid (15 ml)
  8. additionthe pH adjusted to 2 by addition of 2 N sodium hydroxide

出典と根拠

ORDレコード
ord-56a4b015893047a89ea4abb5f019fa9d
出典データセット
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03950376

反応ノート

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