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Dimethylamine → 5-bromo-2-iodo-N,N-dimethylbenzamide

HRID 1865655
ノート
印刷プレビュー

反応式

HRID 1865655 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:11])=[C:6]([CH:10]=1)[C:7](O)=[O:8].[CH3:12][NH:13][CH3:14].C(N(C(C)C)CC)(C)C.C(OCC)(=O)C>CN(C)C=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:11])=[C:6]([CH:10]=1)[C:7]([N:13]([CH3:14])[CH3:12])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 674DimethylamineHCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 3029395-Bromo-2-iodobenzoic acid

生成物 1

HCID 524394945-bromo-2-iodo-N,N-dimethylbenzamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

O-(7-Azabenzotriazol-1-yl)-N,N,N′,N-tetramethyluronium hexafluorophosphate (1.16 g, 3.06 mmol) was added to a solution of 5-bromo-2-iodo-benzoic acid (1.00 g, 3.06 mmol), dimethyl amine (2 M in THF, 3.06 ml, 3.06 mmol) and di-iso-propyl ethyl amine (1.59 ml, 9.18 mmol) in N,N-Dimethylformamide (12 ml). The reaction was stirred at room temperature overnight. Ethyl acetate was added and the mixture was washed with water, the organic layer was dried over magnesium sulfate and evaporated. The residue was purified by silica gel chromatography to yield 5-bromo-2-iodo-N,N-dimethyl-benzamide as a white solid. (0.96 g, 90%). MS: m/z 328.1 (M+H+).

後処理

  1. washthe mixture was washed with water
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. customevaporated
  4. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-35a3429b393a4dac990c3c9ad396e214
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07626021B2

反応ノート

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