Triethylamine → HCID 178488163、化合物

HRID 357553ノート

反応式

HRID 357553 の反応式
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12][C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:15]=3[N:14]=2)[C:6]=1[CH3:24].ClC1C=CC=C(C(OO)=[O:33])C=1.C(N(CC)CC)C.C(=O)([O-])O.[Na+]>CO.ClCCl>[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12]([C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:15]=3[N:14]=2)=[O:33])[C:6]=1[CH3:24]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 178488131HCID 178488131、化合物

生成物 1

HCID 178488163HCID 178488163、化合物収率 61.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

0.9 g of 2-[4-(2-hydroxyethoxy)-3-methylpyridine-2-yl]methylthio-5-methoxy-1H-benzimidazole was dissolved in a mixture comprising 5 ml of methanol and 80 ml of dichloromethane to obtain a solution. 0.51 g of m-chloroperbenzoic acid was added to this solution at -60° C. The obtained mixture was stirred at -50° to -40° C. for 4.5 hours, followed by the addition of 0.38 g of triethylamine. A saturated aqueous solution of sodium hydrogencarbonate was added to the obtained mixture and the resulting mixture was extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was distilled under a reduced pressure to obtain a crude product. This crude product was crystallized from dichloromethane/isopropyl ether to obtain 0.58 g of the title compound.

後処理

  1. customto obtain a solution
  2. extractionthe resulting mixture was extracted with chloroform
  3. dry with materialThe extract was dried over magnesium sulfate
  4. filtrationfiltered
  5. distillationThe filtrate was distilled under a reduced pressure
  6. customto obtain a crude product
  7. customThis crude product was crystallized from dichloromethane/isopropyl ether

出典と根拠

ORDレコード
ord-99f97f5a9dbe4073863cc3e493b3f8a4
出典データセット
uspto-grants-1998_11
特許番号
US05840910

反応ノート

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