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Triethylamine → HCID 178449016、化合物

HRID 1441689
ノート
印刷プレビュー

反応式

HRID 1441689 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:21][CH2:22][CH2:23][CH3:24])[CH2:11][CH2:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[CH:15][CH:14]=1.Cl.[NH2:26][OH:27].C(N(CC)CC)C.C(OCC)(=O)C>O1CCCC1.CO>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:21][CH2:22][CH2:23][CH3:24])[CH2:11][CH2:12][C:13]1[CH:14]=[CH:15][C:16]([C:17]([NH:26][OH:27])=[NH:18])=[CH:19][CH:20]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 443297Hydroxyamine hydrochlorideHCID 591645944-[2-(Benzooxazol-2-yl-butyl-amino)-ethyl]-benzonitrile

生成物 1

HCID 178449016HCID 178449016、化合物収率 87.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

290 mg 4-[2-(Benzooxazol-2-yl-butyl-amino)-ethyl]-benzonitrile were dissolved in a mixture of 10 ml tetrahydrofuran and 20 ml methanol. 930 mg hydroxylamine hydrochloride were added followed by the addition of 2.24 ml triethylamine. The reaction mixture was stirred at 65° C. for two hours. The cooled reaction mixture was diluted by the addition of 100 ml ethyl acetate, then washed three times with 40 ml water. The organic layer was dried over MgSO4, then the solvent was removed in vacuo to obtain 280 mg 4-[2-(Benzooxazol-2-yl-butyl-amino)-ethyl]-N-hydroxy-benzamidine as a pale yellow oil.

後処理

  1. customThe cooled reaction mixture
  2. washwashed three times with 40 ml water
  3. dry with materialThe organic layer was dried over MgSO4
  4. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-bef0f04c489748a8807e6bf86835fa51
出典データセット
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07655679B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート