Methyl iodide → 4-(diphenylmethyl)-1-N-(n-dodecyliminomethyl)piperidine fumarate

HRID 1413950ノート

反応式

HRID 1413950 の反応式
[C:1]1([CH:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:8]2[CH2:13][CH2:12][N:11]([CH:14]=S)[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CI.[CH2:24]([NH2:36])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35].[OH-].[Na+].[C:39]([O-:46])(=[O:45])/[CH:40]=[CH:41]/[C:42]([O-:44])=[O:43]>C(Cl)(Cl)Cl>[C:39]([OH:46])(=[O:45])/[CH:40]=[CH:41]/[C:42]([OH:44])=[O:43].[C:1]1([CH:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:8]2[CH2:13][CH2:12][N:11]([CH:14]=[N:36][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

7

反応物 5

HCID 6328Methyl iodideHCID 13583DodecylamineHCID 14798Sodium HydroxideHCID 5460307FumarateHCID 130978784-(Diphenylmethyl)-1-piperidinecarbothioaldehyde

生成物 1

HCID 202912264-(diphenylmethyl)-1-N-(n-dodecyliminomethyl)piperidine fumarate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A solution of 5.54 g (0.019 mole) of 4-(diphenylmethyl)-1-piperidinecarbothioaldehyde in 20 ml of chloroform was treated with 2.65 g (1.16 ml, 0.019 mole) of methyl iodide and refluxed for one hour. The resulting solution was treated with 3.49 g (0.019 mole) of n-dodecylamine, refluxed one and one half hours, cooled, treated with aqueous sodium hydroxide and the organic layer separated. After drying, evaporation yielded an oil which was converted to the fumarate to yield 4-(diphenylmethyl)-1-N-(n-dodecyliminomethyl)piperidine fumarate; m.p. 143°-145.5° C.

後処理

  1. temperaturerefluxed for one hour
  2. temperaturerefluxed one and one half hours
  3. temperaturecooled
  4. customthe organic layer separated
  5. customAfter drying
  6. customevaporation
  7. customyielded an oil which

出典と根拠

ORDレコード
ord-0d6cffce02a649ea93587ddd40a8a621
出典データセット
uspto-grants-1981_02
特許番号
US04251655

反応ノート

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