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Sodium Chloride → 1-(tert-butyl)-3-((5-chloro-3-(chloromethyl)pyridin-2-yl)methyl)-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one

HRID 706397
ノート
印刷プレビュー

反応式

HRID 706397 の反応式
[C:1]([N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[CH:7]([CH2:14][C:15]2[C:20]([CH2:21]O)=[CH:19][C:18]([Cl:23])=[CH:17][N:16]=2)[C:6]1=[O:24])([CH3:4])([CH3:3])[CH3:2].CN(C=O)C.S(Cl)([Cl:32])=O.[Na+].[Cl-]>ClCCl>[C:1]([N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[CH:7]([CH2:14][C:15]2[C:20]([CH2:21][Cl:32])=[CH:19][C:18]([Cl:23])=[CH:17][N:16]=2)[C:6]1=[O:24])([CH3:4])([CH3:3])[CH3:2]
参加物反応条件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 5234Sodium ChlorideHCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 717382771-(tert-butyl)-3-((5-chloro-3-(hydroxymethyl)pyridin-2-yl)methyl)-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one

生成物 1

HCID 717382761-(tert-butyl)-3-((5-chloro-3-(chloromethyl)pyridin-2-yl)methyl)-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one収率 94.8%

試薬・触媒・溶媒

1
HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 56 (5.8 g, 16.8 mmol) in dichloromethane (30 mL) was added DMF (60 μL) and thionyl chloride (2.2 g) at 5° C. The mixture was stirred for 30 min at this temperature followed by addition of 5% aqueous NaCl (30 mL). The organic layer was separated and washed with 5% aqueous NaCl (30 mL). The solvent was removed and the residue was dissolved in heptane (20 mL). The solution was stirred for 30 min and the product was precipitated. The suspension was cooled to 0° C. and filtered to give 57 (5.8 g, 93%) as a solid:

後処理

  1. customThe organic layer was separated
  2. washwashed with 5% aqueous NaCl (30 mL)
  3. customThe solvent was removed
  4. dissolutionthe residue was dissolved in heptane (20 mL)
  5. stirringThe solution was stirred for 30 min
  6. customthe product was precipitated
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-d51b4624f36d4d008e1258338165c4e4
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09174989B2

反応ノート

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