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Triethylamine → HCID 178495911、化合物

HRID 747542
ノート
印刷プレビュー

反応式

HRID 747542 の反応式
[CH3:1][O:2][CH2:3][CH2:4][NH:5][C:6]1[C:7]([CH3:19])=[C:8]([CH:12]=[CH:13][C:14]=1[S:15]([CH3:18])(=[O:17])=[O:16])[C:9]([OH:11])=O.[OH:20][C:21]1[N:25]([CH3:26])[N:24]=[C:23]([CH:27]2[CH2:29][CH2:28]2)[CH:22]=1.[CH3:30]CN=C=NCCCN(C)C.CCN(CC)CC.[Si](C#N)(C)(C)C.[C-]#N.[K+]>CC#N>[CH:27]1([C:23]2[C:22]([C:9]([C:8]3[CH:12]=[CH:13][C:14]([S:15]([CH3:18])(=[O:17])=[O:16])=[C:6]([N:5]([CH2:4][CH2:3][O:2][CH3:1])[CH3:30])[C:7]=3[CH3:19])=[O:11])=[C:21]([OH:20])[N:25]([CH3:26])[N:24]=2)[CH2:29][CH2:28]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 8471TriethylamineHCID 9032Potassium CyanideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 82115Trimethylsilyl cyanideHCID 691167263-[(2-Methoxyethyl)amino]-2-methyl-4-(methylsulfonyl)benzoic acidHCID 178481725HCID 178481725、化合物

生成物 1

HCID 178495911
HCID 178495911、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Under nitrogen, 0.59 g of crude 3-[(2-methoxyethyl)amino]-2-methyl-4-(methylsulfonyl)benzoic acid was dissolved in 30 ml of CH3CN, and 0.35 g (3 mmol) of 5-hydroxy-3-cyclopropyl-1-methylpyrazole and 0.45 g (2 mmol) of EDAC were then added. The mixture was stirred at RT for one day. 0.36 g (4 mmol) of NEt3, 0.08 g (1 mmol) of Me3SiCN and a spatula tip of KCN were then added, and the mixture was stirred at RT for two days. The mixture was then concentrated, and the residue was taken up in 100 ml of CH2Cl2 and washed with 10% strength H2SO4. The organic phase was dried over MgSO4, concentrated and the residue was purified chromatographically (SiO2, EA/n-heptane=1:1+5% acetic acid). This gave a brown oil.

後処理

  1. stirringthe mixture was stirred at RT for two days
  2. concentrationThe mixture was then concentrated
  3. washwashed with 10% strength H2SO4
  4. dry with materialThe organic phase was dried over MgSO4
  5. concentrationconcentrated
  6. customthe residue was purified chromatographically (SiO2, EA/n-heptane=1:1+5% acetic acid)
  7. customThis gave a brown oil

出典と根拠

ORDレコード
ord-2efd1ae87ab44b23846c95781fa36380
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07396939B2

反応ノート

読み込み中…

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