Hydrochloric Acid → 8-Quinolinol, 5-(chloromethyl)-, hydrochloride (1:1)

HRID 573971

反応式

HRID 573971 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[OH:11])[CH:4]=[CH:3][CH:2]=1.[ClH:12].[CH2:13]=O>O>[ClH:12].[Cl:12][CH2:13][C:6]1[CH:7]=[CH:8][C:9]([OH:11])=[C:10]2[C:5]=1[CH:4]=[CH:3][CH:2]=[N:1]2

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 712FormaldehydeHCID 19238-Hydroxyquinoline

生成物 1

HCID 122695968-Quinolinol, 5-(chloromethyl)-, hydrochloride (1:1)

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 14.6 g (0.1 mol) of 8-quinolinol, 16 mL of 32% HCl in water, and 16 mL (0.1 mL) of 37% formaldehyde in water at 0° C. was treated with hydrogen chloride gas for 6 h. The solution was allowed to stand at room temperature for 2 h without stirring. The yellow solid obtained was collected on a filter, washed with 90% alcohol and dried under vacuum to give 5-chloromethyl-8-quinolinol hydrochloride A (19.0 g, 98%): 1H NMR (250 MHz, CDCl3, δ) 5.32 (s, 2H), 7.53 (m, 1H), 7.85 (m, 2H), 8.12 (m, 1H), 9.12 (m, 1H), 9.28 (m, 1H).

後処理

  1. customThe yellow solid obtained
  2. customwas collected on a filter
  3. washwashed with 90% alcohol
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-208cc568f2f84b298b7cfeefc9fcb376
出典データセット
uspto-grants-2015_05
特許番号
US09034303B2

関連ノート

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