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

HRID 1750273노트

반응식

HRID 1750273 반응식
[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

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 86706952HCID 86706952, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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+].

후처리

  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

출처 및 근거

ORD 기록
ord-bcebf8b53d9c434fa914b4837a4768b4
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156845B2

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