Water → HCID 22033802、化合物

HRID 2163519ノート

反応式

HRID 2163519 の反応式
[C:1]([CH2:4][C:5](=[O:7])[CH3:6])(=[O:3])[CH3:2].C(N(CC)CC)C.[C:15]1([N:21]=[C:22]=[O:23])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.O>C1C=CC=CC=1>[C:1]([CH:4]([C:5](=[O:7])[CH3:6])[C:22]([NH:21][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:23])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 7672Phenyl isocyanateHCID 8471TriethylamineHCID 31261Acetylacetone

生成物 1

HCID 22033802HCID 22033802、化合物収率 73%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A mixture of acetylacetone (5 g) and triethylamine (5.2 g) in dry benzene (50 ml) was treated with phenyl isocyanate (6 g) in dry benzene (25 ml). The mixture was stirred for 3 hr at room temperature. Water (50 ml) was then added, the mixture shaken and the water layer separated. The benzene solution was extracted with two further portions (25 ml) of water and the combined aqueous extracts acidified with dilute hydrochloric acid. The product precipitated and was collected by filtration, washed with water and dried. Diacetyl acetanilide (7.0 g, 73%) was obtained as a colourless solid, m.p. 119-121° C.

後処理

  1. stirringthe mixture shaken
  2. customthe water layer separated
  3. extractionThe benzene solution was extracted with two further portions (25 ml) of water
  4. customThe product precipitated
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-f461f0e1bcd84d2082fefe54d3d0ce03
出典データセット
uspto-grants-1979_01
特許番号
US04134987

反応ノート

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