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Methylamine → 1-(3-Methoxyphenyl)-N-methylethanamine

HRID 1666313
ノート
印刷プレビュー

反応式

HRID 1666313 の反応式
[CH3:1][NH2:2].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:16]=[CH:17][CH:18]=1)[C:8]([C:10]1C=CC=CC=1)=O.[BH4-].[Na+]>CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].O>[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:8]([NH:2][CH3:1])[CH3:10])[CH:16]=[CH:17][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6329MethylamineHCID 4311764Sodium borohydrideHCID 12451863(3-Methoxyphenyl)(phenyl)methanone

生成物 1

HCID 148716881-(3-Methoxyphenyl)-N-methylethanamine

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒HCID 962Water溶媒

実験手順

Titanium(IV) isopropoxide (130 ml) was added to a methanolic methylamine solution (125 ml, 8M) followed by the addition of 3-methoxybenzophenone (50 g). The reaction mixture was stirred at room temperature for 5 hours, after which sodium borohydride (12 g) was carefully added at 0-5° C. The mixture was stirred at room temperature for 2 hours, after which water (60 ml) was added. The inorganic precipitate was filtered off and the filtrate concentrated to dryness. The residue was partitioned between ethyl acetate (400 ml) and aqueous hydrochloric acid (2M, 400 ml). The aqueous phase was made alkaline (pH 11-12) and extracted with dichloromethane (2×300 ml). The organic phase was dried and concentrated to dryness, leaving 1-(3-methoxyphenyl)-N-methylethylamine (43.4 g) as a viscous oil.

後処理

  1. stirringThe mixture was stirred at room temperature for 2 hours
  2. filtrationThe inorganic precipitate was filtered off
  3. concentrationthe filtrate concentrated to dryness
  4. customThe residue was partitioned between ethyl acetate (400 ml) and aqueous hydrochloric acid (2M, 400 ml)
  5. extractionextracted with dichloromethane (2×300 ml)
  6. customThe organic phase was dried
  7. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-d91dfa7fb3724a34919901491a62c8b0
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044067B2

反応ノート

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