Triethylamine → Biotin [2-(4-azidobenzoyl)aminohexyl]amidE

HRID 617683

反応式

HRID 617683 の反応式
[N:1]([C:4]1[CH:19]=[CH:18][C:7]([C:8]([NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]CN)=[O:9])=[CH:6][CH:5]=1)=[N+:2]=[N-:3].[CH2:20]([N:22](CC)CC)C.C1C(=O)N([O:34][C:35]([CH2:37][CH2:38][CH2:39][CH2:40][CH:41]2[S:45][CH2:44][CH:43]3[NH:46][C:47]([NH:49][CH:42]23)=[O:48])=[O:36])C(=O)C1>CN(C=O)C>[OH:36][C:35]([CH2:37][CH2:38][CH2:39][CH2:40][C@H:41]1[C@@H:42]2[C@@H:43]([NH:46][C:47]([NH:49]2)=[O:48])[CH2:44][S:45]1)=[O:34].[N:1]([C:4]1[CH:5]=[CH:6][C:7]([C:8]([NH:10][CH:11]([CH2:12][CH2:13][CH2:14][CH3:15])[CH2:20][NH-:22])=[O:9])=[CH:18][CH:19]=1)=[N+:2]=[N-:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 434213NHS-BiotinHCID 13330101N-(6-Aminohexyl)-4-azidobenzamide

生成物 1

HCID 131721358Biotin [2-(4-azidobenzoyl)aminohexyl]amidE

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
20 °C

実験手順

1.30 g (5 mmol) of product 2b are suspended in 40 ml of distilled DMF and 1.4 ml triethylamine are added under stirring at 20° C. Subsequently, 1.71 g (5 mmol) of biotin-N-hydroxysuccinimide ester 3 are added and stirring is continued for another 3 h at 20° C. Subsequently, the solvent is removed on a rotation evaporator (oil pump vacuum, water bath 50° C.) and the concentrated residue is digested overnight with saturated NaHCO3 solution. Product 4b is drawn off, washed with water and dried in the exsiccator.

後処理

  1. stirringstirring
  2. customSubsequently, the solvent is removed on a rotation evaporator (oil pump vacuum, water bath 50° C.)
  3. waitthe concentrated residue is digested overnight with saturated NaHCO3 solution
  4. washwashed with water
  5. customdried in the exsiccator

出典と根拠

ORDレコード
ord-5565c67d56f746eb8a2c86c07a4205b6
出典データセット
uspto-grants-1999_09
特許番号
US05952185

関連ノート

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