Hydrochloric Acid → 2-[2-(4-Phenylbutyl)phenoxymethyl]morpholine hydrochloride

HRID 743182ノート

反応式

HRID 743182 の反応式
C(OC([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH2:22][CH2:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:9]1)=O)(C)(C)C.[ClH:32]>O1CCOCC1>[ClH:32].[C:26]1([CH2:25][CH2:24][CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:10]2[O:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 106936854-t-Butoxycarbonyl-2-[2-(4-phenylbutyl)phenoxymethyl]morpholine

生成物 1

HCID 194240352-[2-(4-Phenylbutyl)phenoxymethyl]morpholine hydrochloride収率 86%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

671 mg of 4-t-butoxycarbonyl-2-[2-(4-phenylbutyl)phenoxymethyl]morpholine [prepared as described in step (a) above] was dissolved in 10 ml of a 4N solution of hydrogen chloride in dioxane, whilst ice-cooling, and the resulting solution was allowed to stand at room temperature for 30 minutes. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting oily residue was dissolved in 20 ml of ethyl acetate. The solution thus obtained was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 494 mg (yield 86%) of the title compound as colorless crystals, melting at 131°-132° C.

後処理

  1. temperaturecooling
  2. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  3. dissolutionthe resulting oily residue was dissolved in 20 ml of ethyl acetate
  4. customThe solution thus obtained
  5. customto stand at room temperature
  6. customThe crystals which precipitated
  7. filtrationwere collected by filtration
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-5d2dbb9ec4da44e5bf0a3741e7e0f4d6
出典データセット
uspto-grants-1996_09
特許番号
US05556864

反応ノート

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