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Hydrochloric Acid → HCID 20225207、化合物

HRID 1249201
ノート
印刷プレビュー

反応式

HRID 1249201 の反応式
Cl.[C:2]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH:15]([NH:17][CH2:18][CH:19]([O:27][CH3:28])[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=2)[CH3:16])=[CH:10][CH:9]=1)(OC)=[O:3].[CH3:29][NH2:30].Cl>CO.[Cl-].[Na+]>[ClH:26].[CH3:29][NH:30][C:2]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH:15]([NH:17][CH2:18][CH:19]([O:27][CH3:28])[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=2)[CH3:16])=[CH:10][CH:9]=1)=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 6329Methylamine3 回HCID 20225212HCID 20225212、化合物

生成物 1

HCID 20225207HCID 20225207、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 5234Sodium Chloride溶媒

実験手順

To a solution of N-[2-(4-carbomethoxymethoxyphenyl)-1-methylethyl]-2-methoxy-2-(3-chlorophenyl)ethanamine hydrochloride (0.63 g, diastereoisomeric ratio 92:8) in methanol was added 5 ml of a 30% aqueous solution of methylamine. This mixture was boiled under reflux for 6 hours during which time 3 further 5 ml portions of the methylamine solution were added. The solution was cooled to room temperature, a further 5 ml of methylamine solution added and the reaction mixture allowed to stand at room temperature overnight. After diluting with saturated sodium chloride solution the mixture was extracted with dichloromethane, washed with saturated sodium chloride solution, dried (magnesium sulphate), filtered and evaporated to give an oil which was converted to its hydrochloride salt by addition of ethereal hydrogen chloride. Recrystallisation from methanol-ethyl acetate gave the title compound, mp 217°-9° C., as single diastereoisomer.

後処理

  1. additionwere added
  2. extractionwas extracted with dichloromethane
  3. washwashed with saturated sodium chloride solution
  4. dry with materialdried (magnesium sulphate)
  5. filtrationfiltered
  6. customevaporated
  7. customto give an oil which
  8. customRecrystallisation from methanol-ethyl acetate

出典と根拠

ORDレコード
ord-3a2237a7705d44a1b2938630a7c5200b
出典データセット
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04629737

反応ノート

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