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Sodium Sulfite → 2-[(Z)-C-(3-bromophenyl)-N-[(2-methylpropan-2-yl)oxy]carbonimidoyl]-1-oxidopyridin-1-ium-3-ol

HRID 442730
ノート
印刷プレビュー

反応式

HRID 442730 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][CH:21]=1)/[C:5](/[C:12]1[C:17]([OH:18])=[CH:16][CH:15]=[CH:14][N:13]=1)=[N:6]/[O:7][C:8]([CH3:11])([CH3:10])[CH3:9].ClC1C=CC=C(C(OO)=[O:30])C=1.S([O-])([O-])=O.[Na+].[Na+]>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][CH:21]=1)/[C:5](/[C:12]1[C:17]([OH:18])=[CH:16][CH:15]=[CH:14][N+:13]=1[O-:30])=[N:6]/[O:7][C:8]([CH3:11])([CH3:9])[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 135490885(E)-2-(3-bromo-alpha-t-butoxyiminobenzyl)-3-hydroxypyridine

生成物 1

HCID 1364347432-[(Z)-C-(3-bromophenyl)-N-[(2-methylpropan-2-yl)oxy]carbonimidoyl]-1-oxidopyridin-1-ium-3-ol収率 80%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of (Z)-2-(3-bromo-α-t-butoxyiminobenzyl)-3-hydroxypyridine (0.49 g), 70% m-chloroperbenzoic acid (0.70 g) and tetrahydrofuran (30 mL) was stirred overnight at room temperature. To the reaction mixture was added an aqueous solution of sodium sulfite. The reaction mixture was stirred for 30 minutes, and extracted with ethyl acetate. The extract was washed with water and a saturated aqueous saline solution, successively, and dried (sodium sulfate) and then concentrated. The concentrate was crystallized from isopropyl ether, and recrystallized from ethanol-water to afford (Z)-2-(3-bromo-α-t-butoxyiminobenzyl)-3-hydroxypyridine 1-oxide (0.41 g) (compound 3). In substantially the same manner as above, compounds 4, 7, 8, 11, 12 and 15 were produced.

後処理

  1. stirringThe reaction mixture was stirred for 30 minutes
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materiala saturated aqueous saline solution, successively, and dried (sodium sulfate)
  5. concentrationconcentrated
  6. customThe concentrate was crystallized from isopropyl ether
  7. customrecrystallized from ethanol-water

出典と根拠

ORDレコード
ord-78d0cdbe93ec4f1d9b058afdc5fef559
出典データセット
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05891895

反応ノート

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