Hydrochloric Acid → 4-{[(Benzyloxy)carbonyl]amino}-2-hydroxybenzoic acid

HRID 733503

반응식

HRID 733503 반응식
[Na].[NH2:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6](=[CH:10][CH:11]=1)[C:7]([O-:9])=[O:8].Cl[C:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15].Cl>[OH-].[Na+]>[CH2:17]([O:16][C:14]([NH:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[C:5]([OH:12])[CH:4]=1)=[O:15])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10387Benzyl chloroformateHCID 178507646HCID 178507646, 화합물

생성물 1

HCID 2460304-{[(Benzyloxy)carbonyl]amino}-2-hydroxybenzoic acid수율 69.1%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

To a solution of sodium-p-aminosalicylate (100 g, 0.65 mol) in 10% aqueous NaOH solution (1 L) was added a 50% wt solution of benzyl chloroformate (670 g, 1.96 mol in toluene) at 0° C. and stirred at rt for 48 h. The reaction mixture was cooled and acidified with a 10% aqueous HCl at 0° C. The solid obtained was filtered and washed with cold water and dried. The solid was treated with PetEther and filtered to give the title compound (129 g, 68%) used in the next steps without further purification.

후처리

  1. temperatureThe reaction mixture was cooled
  2. customThe solid obtained
  3. filtrationwas filtered
  4. washwashed with cold water
  5. customdried
  6. additionThe solid was treated with PetEther
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-8781117e63c04513a618de00140ecccb
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07589232B2

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