Hydrochloric Acid → 2-Methoxy-5-methylsulfonamidobenzoic Acid

HRID 637193노트

반응식

HRID 637193 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium Hydroxide2회HCID 12848748HCID 12848748, 화합물

생성물 1

HCID 128487462-Methoxy-5-methylsulfonamidobenzoic Acid

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-73786a0e8ca1432ca8f0ee2cf7bb7f07
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194406B1

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