Triethylamine → 2,2,2-Triphenylacetohydrazide

HRID 349169ノート

反応式

HRID 349169 の反応式
[C:1]1([C:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8](O)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.F[P-](F)(F)(F)(F)F.FC(N(C)C)=[N+](C)C.C(N(CC)CC)C.O.[NH2:46][NH2:47]>CN(C)C=O.O>[C:1]1([C:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([NH:46][NH2:47])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 68992Triphenylacetic acidHCID 2774761Tetramethylfluoroformamidinium hexafluorophosphate

生成物 1

HCID 153699862,2,2-Triphenylacetohydrazide収率 65%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

Triphenylacetic acid (499.6 mg, 1.73 mmol) was dissolved in N,N-dimethylformamide (DMF, 3.46 mL). Fluoro-N,N,N′,N′-tetramethylformamidinium hexafluorophosphate (TFFH, 460.1 mg, 1.742 mmol) and anhydrous triethylamine (480 μl, 3.44 mmol) were added and the solution was cooled to 0° C. After 10 minutes hydrazine monohydrate (168 μl, 3.46 mmol) was added. The reaction was allowed to warm, and after stirring at room temperature for 30 minutes, it was worked up by adding water and filtering the resulting precipitate. The precipitate was dried under vacuum to give 2,2,2-triphenylacetohydrazide (340.1 mg).

後処理

  1. temperatureto warm
  2. filtrationfiltering the resulting precipitate
  3. customThe precipitate was dried under vacuum

出典と根拠

ORDレコード
ord-0e9c49cf87154fe1b840c06a4595de6a
出典データセット
uspto-grants-2007_02
特許番号
US07179802B2

反応ノート

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