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Methanesulfonyl chloride → 1-(2,4-Dimethoxypyrimidin-5-yl)-N,N-diethyl-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-amine

HRID 1628664
ノート
印刷プレビュー

反応式

HRID 1628664 の反応式
[CH2:1]([N:3]([CH2:28][CH3:29])[C:4]1[C:9]2[N:10]([CH2:24][CH2:25][CH2:26]O)[C:11]([NH:13][C:14]3[C:15]([O:22][CH3:23])=[N:16][C:17]([O:20][CH3:21])=[N:18][CH:19]=3)=[N:12][C:8]=2[CH:7]=[CH:6][CH:5]=1)[CH3:2].CS(Cl)(=O)=O.C(=O)(O)[O-].[Na+]>N1C=CC=CC=1>[CH3:21][O:20][C:17]1[N:16]=[C:15]([O:22][CH3:23])[C:14]([N:13]2[C:11]3=[N:12][C:8]4[C:9](=[C:4]([N:3]([CH2:1][CH3:2])[CH2:28][CH3:29])[CH:5]=[CH:6][CH:7]=4)[N:10]3[CH2:24][CH2:25][CH2:26]2)=[CH:19][N:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 68762386HCID 68762386、化合物

生成物 1

HCID 577861541-(2,4-Dimethoxypyrimidin-5-yl)-N,N-diethyl-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-amine収率 58.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 3-{7-(diethylamino)-2-[(2,4-dimethoxypyrimidin-5-yl)amino]-1H-benzimidazol-1-yl}propan-1-ol (Reference Example 97; 90 mg, 0.224 mmol) in pyridine (2.0 mL) was added methanesulfonyl chloride (0.035 mL, 0.449 mmol) at 0° C. The mixture was warmed to room temperature and stirred for 3 hr. Aqueous sodium bicarbonate was added and the mixture was extracted with ethyl acetate. Organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give a solid, which was recrystallized from n-hexane/ethyl acetate to give the title compound (50 mg, 0.131 mmol, 58%) as a pale brown solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washOrganic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customto give a solid, which
  6. customwas recrystallized from n-hexane/ethyl acetate

出典と根拠

ORDレコード
ord-9cd71d522e054ba7b1293685fd9e9e56
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785460B2

反応ノート

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