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Hydrochloric Acid → 2,5-Dichlorobenzeneacetic acid

HRID 2043717
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HRID 2043717 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1CC#N.[OH-:12].[Na+].Cl.[CH2:15]([OH:17])[CH3:16]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:16][C:15]([OH:12])=[O:17]
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참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 35312002,5-Dichlorobenzyl cyanide

생성물 1

HCID 947882,5-Dichlorobenzeneacetic acid

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온도
140 °C

실험 절차

A mixture of 2,5-dichlorobenzyl bromide (5.4 g, 22.5 mmol) in 16 mL of ethanol and potassium cyanide (1.63 g, 25 mmol) in 4 mL of water was heated at 80° C. overnight, then cooled, and the solids were filtered and washed with ethanol to give 3.5 g of 2,5-dichlorophenylacetonitrile as a white powder melting at 89-91° C. The nitrile was suspended in 20 red, of ethanol, and 20 mL of a 25% aqueous NaOH solution was added. The mixture was heated in a CEM Explore™ microwave reactor at 140° C. for 30 minutes, then cooled, poured into ice water and acidified to pH 1 with concentrated HCl to give a precipitate. The precipitate was filtered, washed with water and dried in a vacuum oven at 90° C. for 5 h to give the title compound as a white powder.

후처리

  1. temperaturecooled
  2. customto give a precipitate
  3. filtrationThe precipitate was filtered
  4. washwashed with water
  5. customdried in a vacuum oven at 90° C. for 5 h

출처 및 근거

ORD 기록
ord-0a359b494ee54d9998480998a5f78fdb
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586611B2

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