Diphenylmethane → HCID 57269183、化合物

HRID 726530ノート

反応式

HRID 726530 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 57269183HCID 57269183、化合物収率 68%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-6e89d2b9eb18404d827b73c639cdde4c
出典データセット
uspto-grants-1998_01
特許番号
US05710138

反応ノート

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