Hydrochloric Acid → Phosphonic acid, (p-acetamidophenyl)-

HRID 1451058ノート

反応式

HRID 1451058 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([P:8](=[O:11])([OH:10])[OH:9])=[CH:4][CH:3]=1.C(=O)(O)[O-].[Na+].[C:17](OC(=O)C)(=[O:19])[CH3:18].Cl>O>[C:17]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([P:8](=[O:10])([OH:9])[OH:11])=[CH:4][CH:3]=1)(=[O:19])[CH3:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic Anhydride2 回HCID 53590P-(4-Aminophenyl)phosphonic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 155214Phosphonic acid, (p-acetamidophenyl)-収率 38.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a suspension of (4-aminophenyl)phosphonic acid (Aldrich, 0.00058 mol) in water (1.5 mL) was added sufficient sodium bicarbonate to make a clear solution. To the mixture, acetic anhydride (0.2 mL, 0.002 mol) was added and stirred for 0.5 h. Again, acetic anhydride (0.2 mL, 0.002 mol) was added and stirred for 0.5 h. The mixture was let stand at room temperature for 2 h and then concentrated hydrochloric acid (0.5 mL) was added. Fine white needles separated out which were collected by filtration, washed with water and dried to give 0.048 g (38.5%) of the title compound, mp 228° C. (rep. mp 229° C.--Bauer, H. J. Am. Chem. Soc. 1947, 63, 2137-2138).

後処理

  1. stirringstirred for 0.5 h
  2. customat room temperature
  3. customfor 2 h
  4. customFine white needles separated out which
  5. filtrationwere collected by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-c569f7cd0cf84707af9a61fa029e1fb9
出典データセット
uspto-grants-1997_02
特許番号
US05602277

反応ノート

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