Triethylamine → HCID 178488163, 화합물

HRID 727897노트

반응식

HRID 727897 반응식
[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]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 178488131HCID 178488131, 화합물

생성물 1

HCID 178488163HCID 178488163, 화합물수율 61.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1aa50fa7f1eb492e89c88ae880871e82
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05045552

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