Hydrochloric Acid → 2-Methoxy-5-methylsulfonamidobenzoic Acid

HRID 323459ノート

反応式

HRID 323459 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([NH:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:9][C:4]=1[C:5]([O:7]C)=[O:6].[OH-].[Li+].Cl>O1CCCC1.O>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([NH:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:9][C:4]=1[C:5]([OH:7])=[O:6]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium Hydroxide2 回HCID 12848748HCID 12848748、化合物

生成物 1

HCID 128487462-Methoxy-5-methylsulfonamidobenzoic Acid

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

Combine methyl 2-methoxy-5-methylsulfonamidobenzoate (1.0 g, 3.86 mmol) and lithium hydroxide (93 mg, 3.86 mmol) in tetrahydrofuran/water (50 mL/10 mL). After 18 hours, add lithium hydroxide (100 mg) and heat to reflux. After 1 hour, cool to ambient temperature and evaporate to remove most of the tetrahydrofuran. Dilute the evaporated reaction mixture with water (about 70 mL) and acidify to pH of about 1 using a 1 M aqueous hydrochloric acid solution. Evaporate to dryness and triturate with dichloromethane (200 mL). filter and evaporate the filtrate to give the title compound: mp; 160-163° C.

後処理

  1. temperatureheat to reflux
  2. waitAfter 1 hour
  3. customevaporate
  4. customto remove most of the tetrahydrofuran
  5. additionDilute
  6. customthe evaporated reaction mixture with water (about 70 mL)
  7. customEvaporate to dryness
  8. customtriturate with dichloromethane (200 mL)
  9. filtrationfilter
  10. customevaporate the filtrate

出典と根拠

ORDレコード
ord-f0675527dcf14451ba9930a1a49ec128
出典データセット
uspto-grants-2001_04
特許番号
US06211199B1

反応ノート

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