Diphenylphosphinic chloride → HCID 9908920, 화합물

HRID 1458293노트

반응식

HRID 1458293 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 9908920HCID 9908920, 화합물수율 87.4%

시약·촉매·용매 2

HCID 6212Chloroform용매2회HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0f04536133ba4aacbd4d438ea0cc9951
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849930

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