Hydrochloric Acid → HCID 6914595、化合物

HRID 892284ノート

反応式

HRID 892284 の反応式
[OH:1][C:2]1[C:3]([N+:18]([O-:20])=[O:19])=[C:4]([CH:13]=[CH:14][C:15]=1[O:16]C)[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:6].[Cl-].[Al+3].[Cl-].[Cl-].N1C=CC=CC=1.Cl>ClCCCl>[OH:1][C:2]1[C:3]([N+:18]([O-:20])=[O:19])=[C:4]([CH:13]=[CH:14][C:15]=1[OH:16])[C:5]([C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1)=[O:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6451240Aluminum(III) ChlorideHCID 22242329(3-Hydroxy-4-methoxy-2-nitrophenyl)(phenyl)methanone

生成物 1

HCID 6914595HCID 6914595、化合物収率 89%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

To a stirred suspension of 3-Hydroxy4-methoxy-2-nitrobenzophenone (8.3 g, 30.38 mmol) in 1,2-dichloroethane (100 ml) at room temperature under argon was added aluminium chloride (4.46 g, 33.45 mmol) in one portion followed by pyridine (9.61 g, 9.81 ml, 121.5 mmol) giving rise to an exothermic reaction. the mixture was stirred at reflux for one hour, allowed to cool to room temperature and then poured onto ice-water (300 ml). Hydrochloric acid (2N, 70 ml) was added and the mixture was stirred for one hour (initial orange precipitate gradually became yellow in appearance. The solid was removed by filtration, washed by water (30 ml) and dried under vacuum to give the product as a yellow solid 6.99 g, (89%) of melting point 153–155° C. The organic phase of the filtrate was separated and the aqueous phase was extracted by dichloromethane (20 ml). The combined organic phases were washed by brine (30 ml), dried over anhydrous sodium sulphate and the solvent removed on a rotary evaporator (bath temp. 40° C.) to leave a yellow solid (0.7 g) which was not purified further.

後処理

  1. customgiving rise
  2. customto an exothermic reaction
  3. temperatureat reflux for one hour
  4. additionpoured onto ice-water (300 ml)
  5. stirringthe mixture was stirred for one hour (initial orange precipitate gradually became yellow in appearance
  6. customThe solid was removed by filtration
  7. washwashed by water (30 ml)
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-62634ca5dd0643a4ada33ab0e73a0ce5
出典データセット
uspto-grants-2006_02
特許番号
US07005553B2

反応ノート

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