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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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反応

Water → 1-Methyl-3-[3-(4-methyl-1,3-dioxolan-2-yl)-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)uracil

HRID 49006

印刷プレビュー

反応式

HRID 49006 の反応式

[CH3:1][N:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([CH:21]=[O:22])[C:17]=3[CH:23]=2)[C:3]1=[O:24].[CH2:25](O)[CH:26]([OH:28])[CH3:27].C1(C)C=CC=CC=1.O>C(OCC)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:1][N:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([CH:21]4[O:28][CH:26]([CH3:27])[CH2:25][O:22]4)[C:17]=3[CH:23]=2)[C:3]1=[O:24]

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 1030Propylene Glycol

HCID 1140Toluene

HCID 178523685-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1, 2-benzisothiazole-3-carboxaldehyde

生成物 1

HCID 206341811-Methyl-3-[3-(4-methyl-1,3-dioxolan-2-yl)-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)uracil収率 87.6%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxaldehyde (0.500 g, 1.41 mmol), 1,2-propanediol (0.130 ml, 1.83 mmol), p-toluenesulfonic acid (0.0100 g, 0.0100 g, 0.071 mmol) and toluene is stirred at reflux with azeotropic removal of water overnight, cooled to room temperature, diluted with diethyl ether, washed twice with water and once with brine and dried over anhydrous magnesium sulfate. Concentration in vacuo affords a yellow oil, which is chromatographed on silica gel to afford the title compound as a yellow solid (0.510 g, 87.6%, mp 81-83° C.) which is identified by NMR spectral analysis.

後処理

washwashed twice with water and once with brine
dry with materialdried over anhydrous magnesium sulfate
concentrationConcentration in vacuo
customaffords a yellow oil, which
customis chromatographed on silica gel

出典と根拠

ORDレコード: ord-a6c9a94d57604c4a80d996cf7541ff41
出典データセット: uspto-grants-2004_03
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06706663B2

反応ノート

読み込み中…

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