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O-Methylhydroxylamine → 3-{2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-[(methoxyaminocarbonyl)methoxy]pyridine

HRID 1241276
ノート
印刷プレビュー

反応式

HRID 1241276 の反応式
Cl.CN(C)CCCN=C=NCC.[Cl:13][C:14]1[CH:31]=[C:30]([F:32])[C:29]([N:33]2[C:38](=[O:39])[CH:37]=[C:36]([C:40]([F:43])([F:42])[F:41])[N:35]([CH3:44])[C:34]2=[O:45])=[CH:28][C:15]=1[O:16][C:17]1[C:18]([O:23][CH2:24][C:25](O)=[O:26])=[N:19][CH:20]=[CH:21][CH:22]=1.[CH3:46][O:47][NH2:48].C(N(CC)CC)C>O.CN(C)C=O>[CH3:46][O:47][NH:48][C:25](=[O:26])[CH2:24][O:23][C:18]1[C:17]([O:16][C:15]2[CH:28]=[C:29]([N:33]3[C:38](=[O:39])[CH:37]=[C:36]([C:40]([F:41])([F:43])[F:42])[N:35]([CH3:44])[C:34]3=[O:45])[C:30]([F:32])=[CH:31][C:14]=2[Cl:13])=[CH:22][CH:21]=[CH:20][N:19]=1
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 4113O-MethylhydroxylamineHCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 219335233-{2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-carboxymethoxypyridine

生成物 1

HCID 21933566
3-{2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-[(methoxyaminocarbonyl)methoxy]pyridine
収率 28.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

First, 0.13 g of 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride was added to a mixture of 0.30 g of [3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-pyridyloxy]acetic acid (compound a-2), 56 mg of o-methylhydroxylamine, 68 mg of triethylamine, and 2 ml of N,N-dimethylformamide at room temperature, and the mixture was stirred for 2 hours. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and then concentrated. The residue was subjected to silica gel column chromatography to give 90 mg of N-methoxy-[3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-pyridyloxy]acetamide (compound a-104).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-638a96f1716f429da5caf6035662b610
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07115544B2

反応ノート

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