Toluene → HCID 13090781, 화합물

HRID 1252651노트

반응식

HRID 1252651 반응식
[Cl:1][C:2]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([C:10]([N+:13]([O-:15])=[O:14])=[CH:11][CH:12]=1)[CH2:8]O.C1(C)C=CC=CC=1.S(Cl)([Cl:33])=O>N1C=CC=CC=1>[Cl:1][C:2]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([C:10]([N+:13]([O-:15])=[O:14])=[CH:11][CH:12]=1)[CH2:8][Cl:33]

참가 물질

5

반응물 3

HCID 1140TolueneHCID 24386Thionyl ChlorideHCID 13050461HCID 13050461, 화합물

생성물 1

HCID 13090781HCID 13090781, 화합물수율 88%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
110 °C

실험 절차

34.8 parts by weight of 3-(2'-chloro-4'-trifluoromethylphenoxy)-6-nitrobenzyl alcohol were suspended in 200 parts by volume of absolute toluene, 8 parts by weight of pyridine were added, and 13.1 parts by weight of thionyl chloride were added dropwise at 0° C. Thereafter the reaction mixture was stirred for a further 2 hours at 110° C., was cooled, and was extracted with 75 parts by volume of 3N hydrochloric acid and with five times 250 parts by volume of water. The organic phase was separated off, dried with magnesium sulfate and concentrated under reduced pressure. 32 parts by weight (88% of theory) of 3-(2'-chloro-4'-trifluoromethylphenoxy)-6-nitrobenzyl chloride were obtained in the form of an initially oily residue which crystallized when triturated with pentane, to give crystals of melting point 55°-60° C.

후처리

  1. additionwere added
  2. temperaturewas cooled
  3. extractionwas extracted with 75 parts by volume of 3N hydrochloric acid and with five times 250 parts by volume of water
  4. customThe organic phase was separated off
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2a5f19be34174316b62d2718c98881f3
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04744812

반응 노트

불러오는 중…