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

HRID 1015577

반응식

HRID 1015577 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3e02bb80784a42de9000b85da69e6e35
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07985772B2

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