Temozolomide → HCID 49870768、化合物

HRID 570932

反応式

HRID 570932 の反応式
[CH3:1][N:2]1[N:11]=[N:10][C:9]2[N:5]([CH:6]=[N:7][C:8]=2[C:12]([NH2:14])=[O:13])[C:3]1=[O:4].Br[CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=O>>[CH3:1][N:2]1[C:3](=[O:4])[N:5]2[CH:6]=[N:7][C:8]([C:12]3[O:13][CH:16]=[C:17]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[N:14]=3)=[C:9]2[N:10]=[N:11]1

参加物

3

反応物 2

HCID 5394TemozolomideHCID 6259Phenacyl bromide

生成物 1

HCID 49870768HCID 49870768、化合物収率 1%

反応条件

温度
130 °C

実験手順

Temozolomide (0.200 g; 1.03 mmol) and 2-bromoacetophenone (0.246 g; 1.24 mmol) were stirred in a sealed tube under nitrogen, and heated to 130° C. for 1 hour. The mixture was cooled, and then concentrated in vacuo before being applied directly to the head of a chromatography column (SiO2) and purified by column chromatography (DCM:MeOH, 5:1), to give the title compound as a yellow powder (0.003 g; 1%). δH (DMSO-d6) 8.97 (1H, s), 8.88 (1H, s), 7.91 (2H, t, J=7.4), 7.50 (2H, t, J=7.4), 7.39 (1H, t, J=7.4), 3.90 (3H, s).

後処理

  1. temperatureThe mixture was cooled
  2. concentrationconcentrated in vacuo
  3. custompurified by column chromatography (DCM:MeOH, 5:1)

出典と根拠

ORDレコード
ord-b539e4404e004055ae843be7b7fe575d
出典データセット
uspto-grants-2015_05
特許番号
US09024018B2

関連ノート

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