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Diisopropylethylamine → HCID 86672807、化合物

HRID 1755136
ノート
印刷プレビュー

反応式

HRID 1755136 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([C:16]2[NH:20][C:19](=[O:21])[C:18]3([CH2:26][CH2:25][N:24]([S:27]([CH2:30][CH2:31][C:32]4[CH:40]=[CH:39][C:35]([C:36]([OH:38])=O)=[CH:34][C:33]=4[CH3:41])(=[O:29])=[O:28])[CH2:23][CH2:22]3)[N:17]=2)[CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=1)[CH2:2][C:3]#[CH:4].Cl.[N:43]([CH2:46][CH2:47][CH2:48][NH:49][CH3:50])=[N+:44]=[N-:45].CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(OCC)(=O)C>[N:43]([CH2:46][CH2:47][CH2:48][N:49]([CH3:50])[C:36](=[O:38])[C:35]1[CH:39]=[CH:40][C:32]([CH2:31][CH2:30][S:27]([N:24]2[CH2:23][CH2:22][C:18]3([N:17]=[C:16]([C:8]4[CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=[C:6]([O:5][CH2:1][CH2:2][C:3]#[CH:4])[CH:7]=4)[NH:20][C:19]3=[O:21])[CH2:26][CH2:25]2)(=[O:28])=[O:29])=[C:33]([CH3:41])[CH:34]=1)=[N+:44]=[N-:45]
参加物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 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86672806HCID 86672806、化合物HCID 86672808(3-Azidopropyl)(methyl)amine hydrochloride

生成物 1

HCID 86672807HCID 86672807、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

4-{2-[2-(3-But-3-ynyloxy-5-trifluoromethyl-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-3-methyl-benzoic acid, (3-azido-propyl)-methyl-amine hydrochloride (15.3 mg, 0.101 mmol) and DIPEA (0.044 ml, 0.255 mmol) were dissolved in DMF (0.400 ml). HATU (0.038 mg, 0.101 mmol) was added and the mixture was stirred at room temperature for one hour. The reaction solution was diluted with ethyl acetate, and the organic layer was then washed with a 1 M aqueous hydrochloric acid solution, an aqueous sodium bicarbonate solution and saline. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by column chromatography (dichloromethane-ethyl acetate) to give N-(3-azido-propyl)-4-{2-[2-(3-but-3-ynyloxy-5-trifluoromethyl-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-3,N-dimethyl-benzamide as a colorless oily substance.

後処理

  1. washthe organic layer was then washed with a 1 M aqueous hydrochloric acid solution
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by column chromatography (dichloromethane-ethyl acetate)

出典と根拠

ORDレコード
ord-c9ba09b9f9c94233ab79eb64e67de4ec
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09169254B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート