Triethyl phosphite → (2-Chloro-5-methoxy-4 nitrobenzyl)-phosphonic acid diethylester

HRID 2279873ノート

反応式

HRID 2279873 の反応式
Br[CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([N+:11]([O-:13])=[O:12])=[CH:5][C:4]=1[Cl:14].ClC1C=C([N+]([O-])=O)C(OC)=CC=1C.ClC1C=C([N+]([O-])=O)C(OC)=CC=1C(Br)Br.[CH2:43]([O:45][P:46]([O:50]CC)[O:47][CH2:48][CH3:49])[CH3:44]>C1(C)C=CC=CC=1>[CH2:43]([O:45][P:46]([CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([N+:11]([O-:13])=[O:12])=[CH:5][C:4]=1[Cl:14])(=[O:50])[O:47][CH2:48][CH3:49])[CH3:44]

参加物

6

反応物 4

HCID 31215Triethyl phosphiteHCID 158645661-Chloro-4-methoxy-2-methyl-5-nitrobenzeneHCID 678139681-(Bromomethyl)-2-chloro-5-methoxy-4-nitrobenzeneHCID 678145601-Chloro-2-dibromomethyl-4-methoxy-5-nitro-benzene2 回

生成物 1

HCID 86697809(2-Chloro-5-methoxy-4 nitrobenzyl)-phosphonic acid diethylester

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 1-Bromomethyl-2-chloro-5-methoxy-4-nitro-benzene, 1-Chloro-4-methoxy-2-methyl-5-nitro-benzene and 1-chloro-2-dibromomethyl-4-methoxy-5-nitro-benzene (Compound 56G, 24 g, 1:015:0.5) in toluene (100 mL) were treated with triethylphosphite (15.6 g, 94.2 mmol) and heated to reflux for 24 hrs. Toluene and triethylphosphite were distilled off under reduced pressure. The residue was treated with hot diisopropyl ether to give 10 g of the required compound as dark yellow crystals.

後処理

  1. temperatureheated
  2. temperatureto reflux for 24 hrs
  3. distillationToluene and triethylphosphite were distilled off under reduced pressure
  4. additionThe residue was treated with hot diisopropyl ether

出典と根拠

ORDレコード
ord-99404d6ffef2434da3fcdc67602480b5
出典データセット
uspto-grants-2015_09
特許番号
US09133224B2

反応ノート

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