Hydrochloric Acid → 3-(2-Benzyloxy-5-bromophenyl)-acrylic acid

HRID 2196781ノート

反応式

HRID 2196781 の反応式
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:14]([Br:17])=[CH:13][C:10]=1[CH:11]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(=O)[CH2:19][C:20]([OH:22])=[O:21].N1CCCCC1.Cl>N1C=CC=CC=1>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:14]([Br:17])=[CH:13][C:10]=1[CH:11]=[CH:19][C:20]([OH:22])=[O:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 8082PiperidineHCID 7330872-(Benzyloxy)-5-bromobenzaldehyde

生成物 1

HCID 46633083-(2-Benzyloxy-5-bromophenyl)-acrylic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2-benzyloxy-5-bromobenzaldehyde (0.10 mol), malonic acid (15.0 g), and piperidine (2.0 ml) in 150 ml of pyridine was first heated at 90° C. for 90 min and subsequently refluxed for 0.5 hrs. After cooling to room temperature, the reaction was poured on a mixture of ice (1 kg) and concentrated aqueous hydrochloric acid (250 ml). The solid material that precipitated after stirring for 2 hrs. was collected by suction and recrystallized from a minimum of boiling methanol.

後処理

  1. temperaturesubsequently refluxed for 0.5 hrs
  2. temperatureAfter cooling to room temperature
  3. customThe solid material that precipitated
  4. customwas collected by suction
  5. customrecrystallized from a minimum of boiling methanol

出典と根拠

ORDレコード
ord-78f4cf4462e84ab8a9b07fb5c04bf87c
出典データセット
uspto-grants-2012_12
特許番号
US08338478B2

反応ノート

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