Potassium Carbonate → HCID 67502537、化合物

HRID 1887200ノート

反応式

HRID 1887200 の反応式
[C:1]([O:5][C:6](=[O:22])[C@@H:7]([N:10]1[C:15](=[O:16])[C:14]2[N:17]=[CH:18][CH:19]=[CH:20][C:13]=2[NH:12][C:11]1=[O:21])[CH2:8][CH3:9])([CH3:4])([CH3:3])[CH3:2].Br[CH2:24][C:25]1[C:29]2[C:30]([CH3:35])=[CH:31][C:32]([CH3:34])=[CH:33][C:28]=2[S:27][N:26]=1.C(=O)([O-])[O-].[K+].[K+]>O>[C:1]([O:5][C:6](=[O:22])[C@@H:7]([N:10]1[C:15](=[O:16])[C:14]2[N:17]=[CH:18][CH:19]=[CH:20][C:13]=2[N:12]([CH2:24][C:25]2[C:29]3[C:30]([CH3:35])=[CH:31][C:32]([CH3:34])=[CH:33][C:28]=3[S:27][N:26]=2)[C:11]1=[O:21])[CH2:8][CH3:9])([CH3:2])([CH3:3])[CH3:4]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 584973913-Bromomethyl-4,6-dimethyl-benzo[d]isothiazoleHCID 67503155HCID 67503155、化合物

生成物 1

HCID 67502537HCID 67502537、化合物収率 99.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 46 mg of (S)-2-(2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl)-butyric acid tert-butyl ester, 41 mg of 3-bromomethyl-4,6-dimethyl-1,2-benzoisothiazole and 111 mg of potassium carbonate is stirred at room temperature for 4 h. The reaction mixture is diluted with water and the product is filtered and washed with water. The isolated solid is purified by flash chromatography on silica gel to give 72 mg (99%) of (S)-2-[1-(4,6-dimethyl-benzo[d]isothiazol-3-ylmethyl)-2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl]-butyric acid tert-butyl ester.

後処理

  1. filtrationthe product is filtered
  2. washwashed with water
  3. customThe isolated solid is purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-29684024931340509b8319ffc0404d0d
出典データセット
uspto-grants-2013_08
特許番号
US08501749B2

反応ノート

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