Hydrochloric Acid → 5,6,7,8-Tetrahydro-3-methoxy5,5,8,8-tetramethyl-2-naphthaldoxime

HRID 1591120ノート

反応式

HRID 1591120 の反応式
[CH3:1][O:2][C:3]1[C:4]([CH:17]=O)=[CH:5][C:6]2[C:7]([CH3:16])([CH3:15])[CH2:8][CH2:9][C:10]([CH3:14])([CH3:13])[C:11]=2[CH:12]=1.[Cl-].[OH:20][NH3+:21].Cl>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[C:4]([CH:17]=[N:21][OH:20])=[CH:5][C:6]2[C:7]([CH3:16])([CH3:15])[CH2:8][CH2:9][C:10]([CH3:14])([CH3:13])[C:11]=2[CH:12]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21645Hydroxylamine HClHCID 147265222-Formyl-5,6,7,8-tetrahydro-3-methoxy-5,5,8,8tetramethylnaphthalene

生成物 1

HCID 867451925,6,7,8-Tetrahydro-3-methoxy5,5,8,8-tetramethyl-2-naphthaldoxime収率 97.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

5 g (20 millimoles) of 5,6,7,8-tetrahydro-3-methoxy-5,5,8,8-tetramethyl-2-naphthaldehyde and 2.1 g (30 millimoles) of hydroxylammonium chloride in 32.5 ml of dry pyridine were refluxed for 2 hours. The mixture was then allowed to cool, poured onto water and acidified with concentrated hydrochloric acid, and the precipitate which had separated out was filtered off under suction and dried to give 5.1 g of 5,6,7,8-tetrahydro-3-methoxy-5,5,8,8-tetramethyl-2-naphthaldoxime of melting point 182°-183° C.

後処理

  1. temperatureto cool
  2. additionpoured onto water
  3. customthe precipitate which had separated out
  4. filtrationwas filtered off under suction
  5. customdried

出典と根拠

ORDレコード
ord-15929f5ef3734c72a477bcdae3ef00a4
出典データセット
uspto-grants-1993_04
特許番号
US05206242

反応ノート

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