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Triethylamine → HCID 658603、化合物

HRID 2070988
ノート
印刷プレビュー

反応式

HRID 2070988 の反応式
Cl.[NH2:2][OH:3].CCN(CC)CC.[C:11]([C:15]1[C:16]([OH:23])=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH:18]=O)([CH3:14])([CH3:13])[CH3:12]>CC#N>[C:11]([C:15]1[C:16]([OH:23])=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH:18]=[N:2][OH:3])([CH3:14])([CH3:13])[CH3:12]
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 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 36786753-tert-Butyl-2-hydroxybenzaldehyde

生成物 1

HCID 658603HCID 658603、化合物収率 92%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirred solution of hydroxylamine hydrochloride (437 mg, 6.3 mmol) in CH3CN at 0° C. was added Et3N and 3-tert-butyl-2-hydroxybenzaldehyde (1.02 g, 5.7 mmol). The reaction mixture was warmed up to room temperature and stirred for 24 h. The solvent was removed and the residue was dissolved in EtOAc and H2O. The layers were separated and the aqueous layer was extracted with EtOAc (2×20 mL). The combined organic layer was washed with brine, dried with Na2SO4 and concentrated under reduced pressure to provide 3-tert-butyl-2-hydroxybenzaldehyde oxime (1.01 g, 92%) as a pale yellow solid.

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in EtOAc
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with EtOAc (2×20 mL)
  5. washThe combined organic layer was washed with brine
  6. dry with materialdried with Na2SO4
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-eee21e5ee85942b8aaf56d8646253965
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08299267B2

反応ノート

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