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Sodium Hydroxide → HCID 66702670, 화합물

HRID 424646
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HRID 424646 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][C:13]1[C:21]2[C:16](=[N:17][CH:18]=[CH:19][CH:20]=2)[S:15][N:14]=1.[OH-].[Na+]>C(O)(=O)C.ClCCl.O>[CH3:12][C:13]1[C:21]2[C:16](=[N:17][CH:18]=[CH:19][CH:20]=2)[S:15][N+:14]=1[O-:9]
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참가 물질

7

반응물 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 124969753-Methyl-[1,2]thiazolo[5,4-b]pyridine

생성물 1

HCID 66702670HCID 66702670, 화합물수율 62%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매
HCID 6344
Dichloromethane
용매

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온도
25 °C

실험 절차

A solution of m-chloroperbenzoic acid (160 mmol) in acetic acid (200 mL) was added dropwise to a solution of 3-methylisothiazolo[5,4-b]pyridine (107 mmol) in dichloromethane (200 mL). The reaction mixture was maintained for 6 h at 25° C. The reaction mixture was diluted with water (100 mL), the pH was adjusted to 8 with 10% sodium hydroxide, and the layers were separated. The aqueous layer was extracted with ethyl acetate (10×100 mL) and the combined organic layers were dried (magnesium sulfate) and concentrated to provide 3-methylisothiazolo[5,4-b]pyridine-N-oxide in 62% yield as a yellow solid.

후처리

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with ethyl acetate (10×100 mL)
  3. dry with materialthe combined organic layers were dried (magnesium sulfate)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d8722a88d67c4afeb471c3007d47c539
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106066B2

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