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Triethylamine → 1-[1-(1-(tert-butoxycarbonyl)piperidin-4-yl)piperidin-4-yl]-3-(methylsulfonyl)-1,3-dihydro-2H-benzimidazol-2-one

HRID 47535
ノート
印刷プレビュー

反応式

HRID 47535 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[CH2:19][CH2:18][CH:17]([N:20]3[C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=4[NH:22][C:21]3=[O:29])[CH2:16][CH2:15]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH3:37][S:38](Cl)(=[O:40])=[O:39].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([N:14]2[CH2:15][CH2:16][CH:17]([N:20]3[C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=4[N:22]([S:38]([CH3:37])(=[O:40])=[O:39])[C:21]3=[O:29])[CH2:18][CH2:19]2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 15839551HCID 15839551、化合物

生成物 1

HCID 227453061-[1-(1-(tert-butoxycarbonyl)piperidin-4-yl)piperidin-4-yl]-3-(methylsulfonyl)-1,3-dihydro-2H-benzimidazol-2-one

試薬・触媒・溶媒 1

HCID 6212
Chloroform
溶媒

実験手順

One (1) g of 1-[1-(1-(tert-butoxycarbonyl)piperidin-4-yl)-piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one (cf. International Publication WO 96/13262) and 0.53 ml of triethylamine were suspended in 30 ml of chloroform. To the suspension 0.29 ml of methanesulfonyl chloride was added, followed by 2 hours' stirring at room temperature. Saturated aqueous sodium hydrogencarbonate solution was added to the reaction liquid, which was then extracted with chloroform. The extract was dried over sodium sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform, chloroform/methanol=19/1) to give 860 mg of 1-[1-(1-(tert-butoxycarbonyl)piperidin-4-yl)piperidin-4-yl]-3-(methylsulfonyl)-1,3-dihydro-2H-benzimidazol-2-one. The product was dissolved in 25 ml of trifluoroacetic acid, stirred for 30 minutes at room temperature and then the trifluoroacetic acid was distilled off. To the residue ether and chloroform were added and whereby obtained crystals were recovered by filtration, to give 860 mg of the title compound.

後処理

  1. extractionwas then extracted with chloroform
  2. dry with materialThe extract was dried over sodium sulfate
  3. concentrationconcentrated
  4. customthe resulting residue was purified by silica gel column chromatography (chloroform, chloroform/methanol=19/1)

出典と根拠

ORDレコード
ord-091081c242494cbcb6af9e3eeff35824
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06699880B1

反応ノート

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