Ethylene Glycol → 2-Hydroxyphenyltriphenylphosphonium bromide

HRID 1686852ノート

反応式

HRID 1686852 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].[C:9]1([P:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(O)CO>[Ni](Cl)Cl.O>[Br-:1].[C:22]1([P+:15]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[OH:8])[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

参加物

6

反応物 3

HCID 174Ethylene GlycolHCID 72442-BromophenolHCID 11776Triphenylphosphine

生成物 1

HCID 573460052-Hydroxyphenyltriphenylphosphonium bromide

試薬・触媒・溶媒 2

HCID 24385Nickel Dichloride触媒HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

10.4 g (0.060 mol) of 2-bromophenol, 17.3 g (0.066 mol) of triphenyl phosphine, 0.65 g (5 mmol) of nickel chloride, and 40 ml of ethylene glycol were put into a separable flask (volume, 200 ml) equipped with a condenser and a stirrer, and reacted with stirring under heat at 160° C. The reaction liquid was cooled, 40 ml of pure water was dropwise added thereto, and the deposited crystal was washed with toluene, taken out through filtration, and dried to obtain triphenyl(2-hydroxyphenyl)phosphonium bromide.

後処理

  1. custom(volume, 200 ml) equipped with a condenser and a stirrer
  2. customreacted
  3. customThe reaction liquid
  4. temperaturewas cooled
  5. washthe deposited crystal was washed with toluene
  6. filtrationtaken out through filtration
  7. customdried

出典と根拠

ORDレコード
ord-fdb418a511e3424880f528e648deee8c
出典データセット
uspto-grants-2012_04
特許番号
US08148831B2

反応ノート

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