Hydrochloric Acid → HCID 68587975、化合物

HRID 2070235ノート

反応式

HRID 2070235 の反応式
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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 61436Stannous chloride dihydrateHCID 68587480HCID 68587480、化合物

生成物 1

HCID 68587975HCID 68587975、化合物収率 63.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5a3950328df34ec788f42cfa1303a1ea
出典データセット
uspto-grants-2012_10
特許番号
US08299301B2

反応ノート

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