Methylamine → (Bis(4-chlorophenyl)methyl)(methyl)amine

HRID 392824

反応式

HRID 392824 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](Cl)[C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[CH3:17][NH2:18]>O1CCCC1.C(OCC)(=O)C>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([NH:18][CH3:17])[C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 6329MethylamineHCID 130784,4'-Dichlorobenzhydryl chloride

生成物 1

HCID 22660951(Bis(4-chlorophenyl)methyl)(methyl)amine収率 67%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4,4′-dichlorobenzhydryl chloride (3.22 g, 11.85 mmol) in a 1.85 M solution of methylamine in tetrahydrofuran (40 ml) was heated at 125° C. in a pressure vessel for 24 h. The cooled reaction mixture was diluted with ethyl acetate, washed with sodium carbonate, brine and dried (magnesium sulfate). Evaporation of the solvent and chromatography of the residue on silica gel (elution toluene-ethyl acetate 8:2) gave 2.12 g (67%) of the title amine as a clear oil. 1HNMR 400 MHz (CDCl3) δ (ppm): 2.57 (3H, s, NCH3), 4.85 (1H, s, CH benzhydryl), 7.0-7.53 (8H, m, aromatics). MS (ESI+) (m/z): 266 (M+H).

後処理

  1. customThe cooled reaction mixture
  2. washwashed with sodium carbonate, brine
  3. dry with materialdried (magnesium sulfate)
  4. customEvaporation of the solvent and chromatography of the residue on silica gel (elution toluene-ethyl acetate 8:2)

出典と根拠

ORDレコード
ord-6d37b2411615427c8fec0ebe4c06b3d7
出典データセット
uspto-grants-2004_10
特許番号
US06803378B2

関連ノート

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