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2-Bromoethanol → N-[(4-chlorophenyl)methyl]-7-(2-hydroxyethyl)-2-(3-hydroxyprop-1-ynyl)-4-oxo-thieno[2,3-b]pyridine-5-carboxamide

HRID 1978942
ノート
印刷プレビュー

反応式

HRID 1978942 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11]([OH:23])=[C:12]3[CH:18]=[C:17]([C:19]#[C:20][CH2:21][OH:22])[S:16][C:13]3=[N:14][CH:15]=2)=[O:9])=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:33][CH2:34][OH:35]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11](=[O:23])[C:12]3[CH:18]=[C:17]([C:19]#[C:20][CH2:21][OH:22])[S:16][C:13]=3[N:14]([CH2:33][CH2:34][OH:35])[CH:15]=2)=[O:9])=[CH:24][CH:25]=1
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

5

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 178522937HCID 178522937、化合物

生成物 1

HCID 6482391N-[(4-chlorophenyl)methyl]-7-(2-hydroxyethyl)-2-(3-hydroxyprop-1-ynyl)-4-oxo-thieno[2,3-b]pyridine-5-carboxamide収率 36%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

To a solution of N-(4-chlorobenzyl)-4-hydroxy-2-(3-hydroxy-1-propynyl)thieno[2,3-b]pyridine-5-carboxamide (Example No. 5) (0.250 g) in DMF (3 mL) is added K2CO3 (0.278 g) and 2-bromoethanol (0.14 mL). The reaction is heated to 100° C. and stirred for 18 h. The reaction mixture is concentrated in vacuo, and the resulting residue is partitioned between H2O (50 mL) and CH2Cl2 (50 mL). The aqueous layer is extracted with CH2Cl2 (3×50 mL). The combined organic layers are dried with MgSO4, filtered, and concentrated in vacuo to give a small amount of starting material. The desired product precipitates out of the aqueous layer as a tan solid. This material is recrystallized from methanol to yield 0.100 g (36%) of the title compound as a tan, crystalline solid.

後処理

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. customthe resulting residue is partitioned between H2O (50 mL) and CH2Cl2 (50 mL)
  3. extractionThe aqueous layer is extracted with CH2Cl2 (3×50 mL)
  4. dry with materialThe combined organic layers are dried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto give a small amount of starting material
  8. customThe desired product precipitates out of the aqueous layer as a tan solid
  9. customThis material is recrystallized from methanol

出典と根拠

ORDレコード
ord-f9c3d22ef0de4901b2a1db329afc21ac
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06239142B1

反応ノート

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