Dichloromethane → HCID 68511467, 화합물

HRID 1929335노트

반응식

HRID 1929335 반응식
[Cl:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[C:3]=1[CH2:4][O:5][C:6]1[CH:12]=[CH:11][C:9]([NH2:10])=[C:8]([N+:13]([O-])=O)[CH:7]=1.[OH-].[Na+].ClCCl>CO.C(O)(=O)C.[Fe]>[Cl:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[C:8]([NH2:13])[C:9]([NH2:10])=[CH:11][CH:12]=1

참가 물질

7

반응물 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 68512351HCID 68512351, 화합물

생성물 1

HCID 68511467HCID 68511467, 화합물수율 87.7%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 887Methanol용매

실험 절차

add 1.75 g of iron powder to a solution of 1.4 g of 4-[(2,6-dichlorobenzyl)oxy]-2-nitroaniline in 80 cm3 of methanol and 7 cm3 of glacial acetic acid. The reaction mixture is refluxed for three hours. The mixture is concentrated under reduced pressure (0.2 kPa). The residue is taken up in 30 cm3 of water and the pH of the suspension thus obtained is adjusted to 10-11 by adding 2N aqueous solution of sodium hydroxide; 350 cm3 of dichloromethane is then added. After vigorous stirring for 15 min, the insoluble matter is filtered. The filtrate is decanted, then the organic phase is dried over magnesium sulphate, filtered and concentrated under reduced pressure (0.2 kPa). We obtain 1.11 g of 4-[(2,6-dichlorobenzyl)oxy]benzene-1,2-diamine in the form of a black resin, which has the following characteristics:

후처리

  1. temperatureThe reaction mixture is refluxed for three hours
  2. concentrationThe mixture is concentrated under reduced pressure (0.2 kPa)
  3. customthe pH of the suspension thus obtained
  4. filtrationthe insoluble matter is filtered
  5. customThe filtrate is decanted
  6. dry with materialthe organic phase is dried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure (0.2 kPa)

출처 및 근거

ORD 기록
ord-7fa367a22c1c4fe5be92e0052149fade
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188078B2

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