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1,3-Dibromopropane → HCID 20061256、化合物

HRID 1085304
ノート
印刷プレビュー

反応式

HRID 1085304 の反応式
[OH:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[N+:16]([O-:18])=[O:17].C(=O)([O-])[O-].[K+].[K+].[Br:25][CH2:26][CH2:27][CH2:28]Br>CC(CC)=O>[Br:25][CH2:26][CH2:27][CH2:28][O:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[N+:16]([O-:18])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 80011,3-DibromopropaneHCID 11430Potassium CarbonateHCID 2311504-Hydroxy-3-nitrobenzophenone

生成物 1

HCID 20061256HCID 20061256、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

4-hydroxy-3-nitrobenzophenone (2.5 g) and 7.1 g of potassium carbonate were suspended in 15 ml methylethylketone. The suspension was stirred under heating with reflux for 30 minutes, added with 1,3-dibromopropane and then heated with reflux for 6 hours. The reaction mixture was cooled down to room temperature, and insoluble substances were removed by filtration. The filtrate was then concentrated, and the resultant precipitate was subjected to silica gel column chromatograph (hexane/ethyl acetate=3.1 (v/v)) for purification; thereby 2.08 g of an oil, 4-(3-bromopropyloxy)-3-nitrobenzophenone, was obtained.

後処理

  1. temperatureunder heating
  2. temperaturewith reflux for 30 minutes
  3. temperatureheated
  4. temperaturewith reflux for 6 hours
  5. custominsoluble substances were removed by filtration
  6. concentrationThe filtrate was then concentrated
  7. customthe resultant precipitate was subjected to silica gel column chromatograph (hexane/ethyl acetate=3.1 (v/v)) for purification

出典と根拠

ORDレコード
ord-91d45b1af358408aa49d05fdd84a0eaa
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05008267

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート