Pyridine → 5-Acetylaminonaphthalene-2-sulfonic acid

HRID 480671

반응식

HRID 480671 반응식
[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]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 84081,6-Cleve's acid2회HCID 5360545Sodium

생성물 1

HCID 2355515-Acetylaminonaphthalene-2-sulfonic acid

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-d48ea52bf46f4dc390b20558ae0dbe8b
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06653321B1

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