Piperazin-2-one → HCID 59639550、化合物

HRID 556655ノート

反応式

HRID 556655 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][C:2]1=[O:7].C[Al](C)C.[F:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[C:14]=1[N:20]1[C:25]2[N:26]=[C:27]([NH:38][CH2:39][C:40](OC)=[O:41])[N:28]=[C:29]([C:30]3[CH:35]=[CH:34][C:33]([F:36])=[CH:32][C:31]=3[CH3:37])[C:24]=2[CH:23]=[CH:22][C:21]1=[O:44]>>[F:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[C:14]=1[N:20]1[C:25]2[N:26]=[C:27]([NH:38][CH2:39][C:40](=[O:41])[N:4]3[CH2:5][CH2:6][NH:1][C:2](=[O:7])[CH2:3]3)[N:28]=[C:29]([C:30]3[CH:35]=[CH:34][C:33]([F:36])=[CH:32][C:31]=3[CH3:37])[C:24]=2[CH:23]=[CH:22][C:21]1=[O:44]

参加物

4

反応物 3

HCID 231360Piperazin-2-oneHCID 16682925TrimethylaluminumHCID 59639612HCID 59639612、化合物

生成物 1

HCID 59639550HCID 59639550、化合物収率 29%

実験手順

Following the general procedure outlined in Example 193, piperazine-2-one (165 mg, 1.65 mmol), trimethylaluminum (0.83 mL, 1.65 mmol) and the product of Example 190 (150 mg, 0.33 mmol) were reacted to give the crude material. Preparative HPLC, eluting with acetonitrile/H2O (10/90, v/v to 90/10, v/v, over 10 min), followed by recrystallization from dichloromethane and hexane, gave the desired product 50 mg (29%). LC-MS: 523.2 (MH+, m/z), 1.68 (Rt, min).

後処理

  1. customto give the crude material
  2. washPreparative HPLC, eluting with acetonitrile/H2O (10/90, v/v to 90/10
  3. customv/v, over 10 min), followed by recrystallization from dichloromethane and hexane

出典と根拠

ORDレコード
ord-3855ae534d6e49d6b6bb4f6afb515525
出典データセット
uspto-grants-2011_11
特許番号
US08058282B2

反応ノート

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