Diphenylphosphinic chloride → HCID 9908920、化合物

HRID 1458293ノート

反応式

HRID 1458293 の反応式
[CH2:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=O)=[CH:14][CH:13]=1)/[CH:2]=[C:3](/[CH2:5][CH2:6][CH:7]=[C:8]([CH3:10])[CH3:9])\[CH3:4].C1(P(Cl)(C2C=CC=CC=2)=O)C=CC=CC=1.[NH2:36][CH:37]1[CH2:41][N:40]([CH2:42][CH3:43])[N:39]([CH2:44][CH3:45])[CH2:38]1>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH2:44]([N:39]1[CH2:38][CH:37]([NH:36][C:16](=[O:18])[C:15]2[CH:14]=[CH:13][C:12]([O:11][CH2:1]/[CH:2]=[C:3](/[CH2:5][CH2:6][CH:7]=[C:8]([CH3:9])[CH3:10])\[CH3:4])=[CH:20][CH:19]=2)[CH2:41][N:40]1[CH2:42][CH3:43])[CH3:45]

参加物

6

反応物 3

HCID 73910Diphenylphosphinic chlorideHCID 5591991,2-Diethyl-4-pyrazolidinamineHCID 123615004-Geranyloxybenzoic acid

生成物 1

HCID 9908920HCID 9908920、化合物収率 87.4%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒2 回HCID 8471Triethylamine溶媒

実験手順

To a solution of 4- geranyloxybenzoic acid (1.10 g) in chloroform (20 ml), triethylamine (1.11 ml) and a solution of diphenylphosphinic chloride (0.95 g) in chloroform (5 ml) were successively added. After the reaction solution was stirred for 30 minutes, 4-amino-1,2-diethylpyrazolidine (0.57 g) was added and then the mixture was stirred at room temperature for one night. The reaction solution was washed with aqueous solution of sodium hydrogencarbonate, dried over sodium sulfate anhydride, and then concentrated under a vacuum. The residue was purified by silica gel column chromatography (chloroform:methanol=20:1) and then recrystallized from n-hexane, thereby yielding 1.39 g (87%) of the aimed compound.

後処理

  1. stirringthe mixture was stirred at room temperature for one night
  2. washThe reaction solution was washed with aqueous solution of sodium hydrogencarbonate
  3. dry with materialdried over sodium sulfate anhydride
  4. concentrationconcentrated under a vacuum
  5. customThe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)
  6. customrecrystallized from n-hexane

出典と根拠

ORDレコード
ord-0f04536133ba4aacbd4d438ea0cc9951
出典データセット
uspto-grants-1998_12
特許番号
US05849930

反応ノート

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