Potassium Carbonate → 2-Acetylamino-4-nitrophenyl beta-hydroxypropyl ether

HRID 1494287ノート

反応式

HRID 1494287 の反応式
[K].[N+:2]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([NH:12][C:13](=[O:15])[CH3:14])[CH:6]=1)([O-:4])=[O:3].Cl[CH2:17][CH:18]([OH:20])[CH3:19].C(=O)([O-])[O-].[K+].[K+]>O.CN(C)C=O>[OH:20][CH:18]([CH3:19])[CH2:17][O:11][C:8]1[CH:9]=[CH:10][C:5]([N+:2]([O-:4])=[O:3])=[CH:6][C:7]=1[NH:12][C:13](=[O:15])[CH3:14]

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 313701-Chloro-2-propanol2 回HCID 3292867Acetamide, N-(2-hydroxy-5-nitrophenyl)-HCID 5462222Potassium

生成物 1

HCID 198274242-Acetylamino-4-nitrophenyl beta-hydroxypropyl ether

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

0.5 mol (117 g) of the potassium salt of 4-nitro-2-acetylaminophenol is introduced into 300 ml of dimethylformamide in a boiling water-bath, with stirring. The mixture is treated with 0.5 mol (47.25 g) of 1-chloropropan-2-ol. With the heating maintained, 0.5 mol (47.25 g) of 1-chloropropan-2-ol and 0.25 mol (34.5 g) of potassium carbonate are added four times at 2-hour intervals. After heating for 10 hours, the reaction mixture is poured into 1,500 ml of iced water. The expected product, which has precipitated, is filtered off. It is washed with a 0.5N solution of sodium hydroxide and then with water. After drying in vacuo at 60° C., it melts at 123° C.

後処理

  1. temperatureWith the heating maintained
  2. temperatureAfter heating for 10 hours
  3. customThe expected product, which has precipitated
  4. filtrationis filtered off
  5. washIt is washed with a 0.5N solution of sodium hydroxide
  6. customAfter drying in vacuo at 60° C.

出典と根拠

ORDレコード
ord-a198e0af87f04cb6a33342bf8c8022d3
出典データセット
uspto-grants-1991_06
特許番号
US05026401

反応ノート

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