2-Aminobenzyl alcohol → (2-Aminobenzyl)triphenylphosphonium bromide

HRID 468371

反応式

HRID 468371 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]O.[BrH:10].[C:11]1([P:17]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(#N)C>[Br-:10].[C:24]1([P+:17]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=2[NH2:1])[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

参加物

4

反応物 2

HCID 214392-Aminobenzyl alcoholHCID 80811Triphenylphosphonium bromide

生成物 1

HCID 10961315(2-Aminobenzyl)triphenylphosphonium bromide収率 88.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-Aminobenzyl alcohol (60.0 g, 0.487 mol) was dissolved in acetonitrile (2.5 L) and brought to reflux. Triphenylphosphine hydrobromide (167 g, 0.487 mol) was added and the mixture was heated at reflux for 3 h. The reaction mixture was concentrated to approximately 500 mL and left at room temperature for 1 h. The precipitate was filtered and washed with cold acetonitrile followed by hexane. The solid was dried overnight at 40° C. under vacuum to give triphenyl(2-aminobenzyl)phosphonium bromide (193 g, 88%).

後処理

  1. temperatureto reflux
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 3 h
  4. concentrationThe reaction mixture was concentrated to approximately 500 mL
  5. filtrationThe precipitate was filtered
  6. washwashed with cold acetonitrile
  7. customThe solid was dried overnight at 40° C. under vacuum

出典と根拠

ORDレコード
ord-d3c011fa54dc49abb7ffd437c3a653c8
出典データセット
uspto-grants-2014_01
特許番号
US08623905B2

関連ノート

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