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Dimethyl-(5-vinyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)amine → (5-Ethyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)dimethylamine

HRID 25336
ノート
印刷プレビュー

反応式

HRID 25336 の反応式
[CH3:1][N:2]([CH3:18])[CH:3]1[C:12]2[CH2:11][O:10][C:9]([CH:13]=[CH2:14])=[CH:8][C:7]3=[CH:15][NH:16][CH:17]=[C:5]([C:6]=23)[CH2:4]1>CO.[H][H].[Pd]>[CH2:13]([C:9]1[O:10][CH2:11][C:12]2[CH:3]([N:2]([CH3:1])[CH3:18])[CH2:4][C:5]3=[CH:17][NH:16][CH:15]=[C:7]([C:6]=23)[CH:8]=1)[CH3:14]
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 1

HCID 69736453Dimethyl-(5-vinyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)amine

生成物 1

HCID 69737167(5-Ethyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)dimethylamine収率 99%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 178418361HCID 178418361、化合物溶媒

実験手順

Compound (40) 242 mg was dissolved in methanol 4 ml and 5% palladium/C 60 mg was added. A mixture was stirred in hydrogen atmosphere at room temperature for 3 h. The catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in ethyl acetate:hexane (1:2) to give the titled compound as colorless crystals 241.6 mg. Yield 99%. This was recrystallized from acetone-hexane to give the titled compound as colorless crystals, m.p. 91-92° C.

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue obtained
  4. customwas chromatographed on aluminum oxide in ethyl acetate:hexane (1:2)

出典と根拠

ORDレコード
ord-da8661081381406dbab38b6ee040d84d
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06858640B2

反応ノート

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