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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Dimethylformamide → Undecylamine

HRID 535115
ノート
印刷プレビュー

反応式

HRID 535115 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12](O)=O.C(N(CC)CC)C.C1C(SSC2C=CC([N+]([O-])=O)=C(C(O)=O)C=2)=CC(C(O)=O)=C([N+]([O-])=O)C=1.CN(C=O)C>O1CCCC1>[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 62545,5'-Dithiobis(2-nitrobenzoic Acid)HCID 8471TriethylamineHCID 1708311-Aminoundecanoic acid

生成物 1

HCID 81742Undecylamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

In this example, the spacer unit is 11-amino-undecanoic acid. The spacer (411 mg, 2.04 mmol, 4 eq) is suspended in a dry organic solvent, for example tetrahydrofuran (THF). Depending on its solubility and the stability of the Raman marker unit, the suspension temperature can be varied between −78° C. and reflux. First, an auxiliary base (2.1 ml triethylamine) is added. Then, the activated marker unit in a suitable organic solvent, for example DTNB-NHS (300 mg, 0.51 mmol in 10 ml THF and 5 ml DMF), is added dropwise. Depending on the reactivity, the reaction mixture is stirred 10 to 48 h, in this case 16 h. The solvent is removed by vacuum, the remaining solid is washed with NaHSO4 solution and a suitable organic solvent. Further purification can be achieved by column chromatography, preferably on reversed phase silica (yield: 260 mg, 0.34 mmol, 67%).

後処理

  1. customcan be varied between −78° C.
  2. temperaturereflux
  3. customThe solvent is removed by vacuum
  4. washthe remaining solid is washed with NaHSO4 solution
  5. customFurther purification

出典と根拠

ORDレコード
ord-23394465a7ce451786c3fbf93ef3ead9
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08854617B2

反応ノート

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