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Water → HCID 86635726、化合物

HRID 1013336
ノート
印刷プレビュー

反応式

HRID 1013336 の反応式
[Cl:1]N1C(=O)CCC1=O.[CH3:9][O:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[CH:14]=[N:15][OH:16].O>CN(C=O)C>[Cl:1][C:13]1([CH:14]=[N:15][OH:16])[CH:17]=[CH:18][CH:19]=[C:11]([O:10][CH3:9])[CH2:12]1
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 962WaterHCID 31398ChlorosuccinimideHCID 293577N-[(3-methoxyphenyl)methylidene]hydroxylamine

生成物 1

HCID 86635726HCID 86635726、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-chlorosuccinimide (32.2 g, 241 mmol) was added to a solution of 3-methoxybenzaldehyde oxime (30.4 g, 201 mmol) in DMF (200 ml) at RT, causing the temperature to rise briefly to 50° C. The reaction mixture was cooled in an ice bath, stirred overnight at RT, mixed with water (250 ml) while being cooled with ice and the precipitate formed was removed by suction-filtration. The filtrate was extracted with ether (3×400 ml) and the combined organic phases were washed with water (300 ml) and sat. aq. NaCl solution (300 ml), dried and the solvent was removed under vacuum. The desired product 1-chloro-1-hydroxyiminomethyl-3-methoxybenzene was obtained as a yellowish solid (32.86 g).

後処理

  1. customto rise briefly to 50° C
  2. temperatureThe reaction mixture was cooled in an ice bath
  3. temperaturewhile being cooled with ice
  4. customthe precipitate formed
  5. customwas removed by suction-filtration
  6. extractionThe filtrate was extracted with ether (3×400 ml)
  7. washthe combined organic phases were washed with water (300 ml) and sat. aq. NaCl solution (300 ml)
  8. customdried
  9. customthe solvent was removed under vacuum

出典と根拠

ORDレコード
ord-c495f19d278b49c9bbdfc663450aeb6a
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981883B2

反応ノート

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