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

HRID 468371

반응식

HRID 468371 반응식
[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

참가 물질

4

반응물 2

HCID 214392-Aminobenzyl alcoholHCID 80811Triphenylphosphonium bromide

생성물 1

HCID 10961315(2-Aminobenzyl)triphenylphosphonium bromide수율 88.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-d3c011fa54dc49abb7ffd437c3a653c8
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623905B2

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