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Diisopropylethylamine → HCID 71238220、化合物

HRID 926085
ノート
印刷プレビュー

反応式

HRID 926085 の反応式
[NH2:1][C:2]1[S:3][C:4]2[CH2:21][CH2:20][CH2:19][CH2:18][C:5]=2[C:6]=1[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=1)=[O:8].[C:22]([N:25]1[CH2:30][CH2:29][N:28]([S:31]([C:34]2[CH:35]=[C:36]([CH:40]=[CH:41][CH:42]=2)[C:37](O)=[O:38])(=[O:33])=[O:32])[CH2:27][CH2:26]1)(=[O:24])[CH3:23].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)C(C)C)(C)C>CC(N(C)C)=O>[C:22]([N:25]1[CH2:30][CH2:29][N:28]([S:31]([C:34]2[CH:35]=[C:36]([CH:40]=[CH:41][CH:42]=2)[C:37]([NH:1][C:2]2[S:3][C:4]3[CH2:21][CH2:20][CH2:19][CH2:18][C:5]=3[C:6]=2[C:7]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)=[O:8])=[O:38])(=[O:32])=[O:33])[CH2:27][CH2:26]1)(=[O:24])[CH3:23]
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 81531DiisopropylethylamineHCID 7228582-amino-N-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamideHCID 24428203-[(4-acetyl-1-piperazinyl)sulfonyl]benzoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 71238220HCID 71238220、化合物
収率 25%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

A mixture of 10.6 mg of 2-amino-N-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide, 10.9 mg of 3-(4-acetyl-piperazine-1-sulfonyl)benzoic acid, 16.0 mg of HATU, 0.012 mL of N,N-diisopropylethylamine, and 1 mL of DMA was stirred at room temperature overnight. The reaction mixture was separated by the addition of chloroform and water, and then the organic layer was concentrated under reduced pressure. The obtained residue was purified by preparative high performance liquid chromatography (methanol-0.1% aqueous formic acid solution) to obtain 5.2 mg of 2-({3-[(4-acetylpiperazin-1-yl)sulfonyl]benzoyl}amino)-N-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide.

後処理

  1. customThe reaction mixture was separated by the addition of chloroform and water
  2. concentrationthe organic layer was concentrated under reduced pressure
  3. customThe obtained residue was purified by preparative high performance liquid chromatography (methanol-0.1% aqueous formic acid solution)

出典と根拠

ORDレコード
ord-708bb0635d584050933594bf2540b2d5
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09284295B2

反応ノート

読み込み中…

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