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

HRID 2279873노트

반응식

HRID 2279873 반응식
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]

참가 물질

6

반응물 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-benzene2회

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-99404d6ffef2434da3fcdc67602480b5
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133224B2

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