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

HRID 902762

反応式

HRID 902762 の反応式
[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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10387Benzyl chloroformateHCID 178507646HCID 178507646、化合物

生成物 1

HCID 2460304-{[(Benzyloxy)carbonyl]amino}-2-hydroxybenzoic acid収率 68.6%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

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 (128 g, 68%) used in the next steps without further purification.

後処理

  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

出典と根拠

ORDレコード
ord-0296863cb5b848208ac8a77cd8b340c4
出典データセット
uspto-grants-2008_04
特許番号
US07365225B2

関連ノート

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