Hydrochloric Acid → HCID 68587975, 화합물

HRID 2070235노트

반응식

HRID 2070235 반응식
O.O.[Sn](Cl)Cl.Cl.[C:7]([C:11]1[CH:12]=[C:13]([CH:29]=[CH:30][CH:31]=1)[O:14][C:15]1[C:20]([C:21]([F:24])([F:23])[F:22])=[CH:19][C:18]([N+:25]([O-])=O)=[C:17]([CH3:28])[CH:16]=1)([CH3:10])([CH3:9])[CH3:8]>CO>[C:7]([C:11]1[CH:12]=[C:13]([CH:29]=[CH:30][CH:31]=1)[O:14][C:15]1[C:20]([C:21]([F:24])([F:22])[F:23])=[CH:19][C:18]([NH2:25])=[C:17]([CH3:28])[CH:16]=1)([CH3:10])([CH3:8])[CH3:9]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 61436Stannous chloride dihydrateHCID 68587480HCID 68587480, 화합물

생성물 1

HCID 68587975HCID 68587975, 화합물수율 63.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Initially, at room temperature, 37.55 g (166.41 mmol) of tin(II) chloride dihydrate and then, with ice-cooling and slowly, 100 ml of concentrated hydrochloric acid are added to a solution of 19.60 g (55.47 mmol) of 4-(3-tertbutylphenoxy)-5-trifluoromethyl-2-methylnitrobenzene in 100 ml of methanol. The mixture is heated under reflux for 4 h, cooled to room temperature, concentrated, water is added and the residue is filtered off and dried under reduced pressure. The crude product is purified by column chromatography. (13.2 g, purity 86%, yield 63.5%, log P (pH 2.3)=4.67).

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 4 h
  3. concentrationconcentrated
  4. additionwater is added
  5. filtrationthe residue is filtered off
  6. customdried under reduced pressure
  7. customThe crude product is purified by column chromatography

출처 및 근거

ORD 기록
ord-5a3950328df34ec788f42cfa1303a1ea
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299301B2

반응 노트

불러오는 중…