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Hydrazine → (E)-N-(6,6-dimethyl-2-hepten-4-ynyl)-N-ethyl-3-aminobenzylamine

HRID 2254471
ノート
印刷プレビュー

反応式

HRID 2254471 の反応式
[CH3:1][C:2]([CH3:30])([CH3:29])[C:3]#[C:4]/[CH:5]=[CH:6]/[CH2:7][N:8]([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([N:18]2C(=O)C3=CC=CC=C3C2=O)[CH:13]=1)[CH2:9][CH3:10].NN>C(O)C>[CH3:29][C:2]([CH3:1])([CH3:30])[C:3]#[C:4]/[CH:5]=[CH:6]/[CH2:7][N:8]([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([NH2:18])[CH:13]=1)[CH2:9][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

4

反応物 2

HCID 9321HydrazineHCID 19744709(E)-N-(6,6-dimethyl-2-hepten-4-ynyl)-N-ethyl-3-phthalimidobenzylamine

生成物 1

HCID 19917001(E)-N-(6,6-dimethyl-2-hepten-4-ynyl)-N-ethyl-3-aminobenzylamine収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

150 mg of the resulting benzylamine compound was dissolved in 5 ml of ethanol, and 23 mg of hydrazine was added. The mixture was stirred at room temperature for 30 minutes. The precipitate was separated by filtration, and the solvent was evaporated. The residue was distributed between methylene chloride and water. The organic layer was worked up in a customary manner and purified by silica gel column chromatography [Wakogel C-100, 5 g; eluting solvent: hexane/ethyl acetate=10/1→3/1] to give 95 mg (yield 95%) of the captioned compound as a pale yellow crystalline powder, m.p. 65°-66 ° C.

後処理

  1. customThe precipitate was separated by filtration
  2. customthe solvent was evaporated
  3. custompurified by silica gel column chromatography [Wakogel C-100, 5 g; eluting solvent: hexane/ethyl acetate=10/1→3/1]

出典と根拠

ORDレコード
ord-91902ca3635e4c3a89bdaaa3e4b59bdb
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05234946

反応ノート

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