Diphenylmethane → HCID 57269183, 화합물

HRID 726530노트

반응식

HRID 726530 반응식
[N+:1]([C:4]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]=1Cl)([O-:3])=[O:2].C1(CC2C=CC=CC=2)C=CC=CC=1.[CH2:31]([O:33][P:34]([CH2:39][NH2:40])(=[O:38])[O:35][CH2:36][CH3:37])[CH3:32]>C(Cl)Cl>[CH2:31]([O:33][P:34]([CH2:39][NH:40][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:12]([N+:14]([O-:16])=[O:15])=[CH:13][C:4]=1[N+:1]([O-:3])=[O:2])(=[O:38])[O:35][CH2:36][CH3:37])[CH3:32]

참가 물질

5

반응물 3

HCID 7580DiphenylmethaneHCID 169871-Chloro-2,4-dinitronaphthaleneHCID 1596920Diethyl (aminomethyl)phosphonate

생성물 1

HCID 57269183HCID 57269183, 화합물수율 68%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4 g of 2,4 dinitro-1-chloronaphthalene (15.84 mmol) is dissolved in 6.5 g of aminomethanephosphonic acid diethyl ester and 4 g of diphenylmethane and stirred for 72 hours at room temperature. The batch is diluted with methylene chloride, washed with 1N NaOH and washed twice with brine, dried and spun in. The crude product is chromatographed on silica gel with 3.5 liters of cyclohexane and ethyl acetate 1:1 as mobile solvent. 68% of product is obtained in several fractions as viscous oil. NMR (DMSO, delta in ppm): 1.15(6H,tr), 4(4H dq)4.25 (2H m), 7.8, 7.98, 8.9, 9.05 each 1H, 8.6 (2H,d)

후처리

  1. washwashed with 1N NaOH
  2. washwashed twice with brine
  3. customdried
  4. customThe crude product is chromatographed on silica gel with 3.5 liters of cyclohexane and ethyl acetate 1:1 as mobile solvent

출처 및 근거

ORD 기록
ord-6e89d2b9eb18404d827b73c639cdde4c
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05710138

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