Trifluoroacetic acid → HCID 20450402、化合物

HRID 358106ノート

反応式

HRID 358106 の反応式
COC1C=CC(C[O:10][C:11]([CH2:13][C:14]([O:16][C:17]2[CH:18]=[C:19]([C:23]3[N:24]=[C:25]4[N:29]([CH:30]=3)[C:28]3[CH:31]=[CH:32][CH:33]=[CH:34][C:27]=3[S:26]4)[CH:20]=[CH:21][CH:22]=2)=[O:15])=[O:12])=CC=1.C1(OC)C=CC=CC=1.FC(F)(F)C(O)=O.C(O)C.[ClH:53]>ClCCl.O1CCCC1>[ClH:53].[C:11]([CH2:13][C:14]([O:16][C:17]1[CH:18]=[C:19]([C:23]2[N:24]=[C:25]3[N:29]([CH:30]=2)[C:28]2[CH:31]=[CH:32][CH:33]=[CH:34][C:27]=2[S:26]3)[CH:20]=[CH:21][CH:22]=1)=[O:15])([OH:12])=[O:10]

参加物

7

反応物 4

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 13206728HCID 13206728、化合物HCID 21887872Ethanol hydrochloride

生成物 1

HCID 20450402HCID 20450402、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 5 ml of anhydrous dichloromethane was dissolved 1.146 g of 2-[m-(p-methoxyphenylmethoxycarbonylacetoxy)phenyl]imidazo[2,1-b]benzothiazole and after adding thereto 0.4 ml of anisole, the mixture was cooled with ice-water. Then, 5 ml of trifluoroacetic acid was added dropwise to the mixture and the resultant mixture was stirred for one hour. The reaction mixture thus formed was concentrated under reduced pressure and the oily product thus obtained was dissolved in 10 ml of anhydrous tetrahydrofuran. Then, while stirring the mixture under ice-cooling, 2 ml of 2N hydrogen chloride ethanol solution was added to the solution and white crystals thus precipitated were recovered by filtration to provide 911 mg of 2-(m-carboxyacetoxyphenyl)imidazo[2,1-b]benzothiazole hydrochloride.

後処理

  1. additionafter adding
  2. customThe reaction mixture thus formed
  3. concentrationwas concentrated under reduced pressure
  4. customthe oily product thus obtained
  5. temperaturecooling
  6. customthus precipitated
  7. filtrationwere recovered by filtration

出典と根拠

ORDレコード
ord-a6d31499b13c4a099b7626e686fd8ee8
出典データセット
uspto-grants-1984_08
特許番号
US04464384

反応ノート

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