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

HRID 392824

반응식

HRID 392824 반응식
[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

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 130784,4'-Dichlorobenzhydryl chloride

생성물 1

HCID 22660951(Bis(4-chlorophenyl)methyl)(methyl)amine수율 67%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-6d37b2411615427c8fec0ebe4c06b3d7
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06803378B2

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