Triphosgene → 1-Bromo-4-(1-isocyanatoethyl)benzene

HRID 1096302ノート

反応式

HRID 1096302 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([NH2:10])[CH3:9])=[CH:4][CH:3]=1.[C:11]([O-])(O)=[O:12].[Na+].ClC(Cl)(OC(=O)OC(Cl)(Cl)Cl)Cl>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:10]=[C:11]=[O:12])[CH3:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 94429TriphosgeneHCID 516892Sodium BicarbonateHCID 852999(alphaS)-4-Bromo-alpha-methylbenzenemethanamine

生成物 1

HCID 6109831-Bromo-4-(1-isocyanatoethyl)benzene収率 63%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (S)-1-(4-bromophenyl)ethanamine (240 g, 1.2 mol) in methylene chloride (3 L) and satd aq NaHCO3 (3 L) solution was added triphosgene (118 g, 0.396 mol) at 0° C. The mixture was stirred for 15 min. The organic phase was separated, dried over Na2SO4 and concentrated to give 1-bromo-4-(1-isocyanato-ethyl)-benzene (170 g, 63%).

後処理

  1. customThe organic phase was separated
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-2bbe12e794a445a784ed2596b7168fc3
出典データセット
uspto-grants-2012_03
特許番号
US08138178B2

反応ノート

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