Potassium Carbonate → 3-(4-chloro-7H-pyrrolo[2,3-d]pyrimidin-5-yl)benzonitrile

HRID 1750273

反応式

HRID 1750273 の反応式
[Cl:1][C:2]1[C:3]2[C:10]([C:11]3[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=3)[C:14]#[N:15])=[CH:9][N:8](CO)[C:4]=2[N:5]=[CH:6][N:7]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:1][C:2]1[C:3]2[C:10]([C:11]3[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=3)[C:14]#[N:15])=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 86706952HCID 86706952、化合物

生成物 1

HCID 867069533-(4-chloro-7H-pyrrolo[2,3-d]pyrimidin-5-yl)benzonitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 3-[4-chloro-7-(hydroxymethyl)-7H-pyrrolo[2,3-d]pyrimidin-5-yl]benzonitrile (C13) (4 g from the previous step, ≦9.9 mmol) in methanol (100 mL) was adjusted to pH>12 by addition of solid potassium carbonate. Solvent was removed in vacuo and the residue was mixed with water (100 mL). The resulting solid was isolated via filtration and washed with water, providing the product as a white solid. Yield: 1.3 g, 5.1 mmol, 52% over two steps. LCMS m/z 255.0 [M+H+].

後処理

  1. customSolvent was removed in vacuo
  2. additionthe residue was mixed with water (100 mL)
  3. customThe resulting solid was isolated via filtration
  4. washwashed with water

出典と根拠

ORDレコード
ord-bcebf8b53d9c434fa914b4837a4768b4
出典データセット
uspto-grants-2015_10
特許番号
US09156845B2

関連ノート

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