Pyridine → 5-Acetylaminonaphthalene-2-sulfonic acid

HRID 480671

反応式

HRID 480671 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([S:12]([OH:15])(=[O:14])=[O:13])=[CH:7]2.N1C=CC=CC=1.[C:22](OC(=O)C)(=[O:24])[CH3:23].[Na]>CO.C(OCC)C>[C:22]([NH:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([S:12]([OH:15])(=[O:13])=[O:14])=[CH:7]2)(=[O:24])[CH3:23]

参加物

7

反応物 4

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 84081,6-Cleve's acid2 回HCID 5360545Sodium

生成物 1

HCID 2355515-Acetylaminonaphthalene-2-sulfonic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 3283Diethyl Ether溶媒

実験手順

To 29.3 g (0.13 mol) of 5-amino-2-naphthalenesulfonic Acid (Compound 72) was added 40 mL of pyridine and 26 mL of acetic anhydride. The resulting suspension was allowed to stir at ambient temperature. After 24 hr, the resulting solution was diluted with 60 mL of methanol. Then, a solution of 3.6 g (0.156 mol) of sodium in 100 mL of methanol was added. After a solid precipitate began to form, 200 mL of diethyl ether was added and the suspension allowed to stir. The solid was collected by vacuum filtration and was washed with diethyl ether. This provided 38.9 g (0.11 mol) of the desired product. The product was identified by 1H NMR and mass spectroscopy and purity was assessed by RP-HPLC.

後処理

  1. customto form
  2. stirringto stir
  3. filtrationThe solid was collected by vacuum filtration
  4. washwas washed with diethyl ether

出典と根拠

ORDレコード
ord-d48ea52bf46f4dc390b20558ae0dbe8b
出典データセット
uspto-grants-2003_11
特許番号
US06653321B1

関連ノート

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