Hydrochloric Acid → 4-(Azetidin-3-yl)morpholine dihydrochloride

HRID 1384797ノート

反応式

HRID 1384797 の反応式
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH2:9]2)C=CC=CC=1.[ClH:24]>[OH-].[Pd+2].[OH-].C(O)C>[ClH:24].[ClH:24].[O:15]1[CH2:16][CH2:17][N:12]([CH:10]2[CH2:11][NH:8][CH2:9]2)[CH2:13][CH2:14]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 211837864-[1-(Diphenylmethyl)azetidin-3-yl]morpholine

生成物 1

HCID 220613264-(Azetidin-3-yl)morpholine dihydrochloride

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

A mixture of 1-diphenylmethyl-3-morpholinoazetidine (prepared in an analogous manner to the compound of preparation 22 above) (18.6 g), palladium hydroxide (2 g), ethanol (200 ml) and 1N aqueous hydrochloric acid solution (52 ml) was stirred under an atmosphere of hydrogen at 345 kPa (50 p.s.i.) for 3 days. The catalyst was then removed by filtration and the filtrate evaporated to dryness. Addition of dichloromethane (100 ml) to the residue and trituration gave a solid which was recrystallised from methanol to give the title compound (10.2 g).

後処理

  1. customThe catalyst was then removed by filtration
  2. customthe filtrate evaporated to dryness
  3. additionAddition of dichloromethane (100 ml) to the residue and trituration
  4. customgave a solid which
  5. customwas recrystallised from methanol

出典と根拠

ORDレコード
ord-7ad0e197b7a94a1fa2a8b5c8fcdc2e0d
出典データセット
uspto-grants-2001_07
特許番号
US06262046B1

反応ノート

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