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Acetone → 2-{6-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyridin-3-yl}-propane-1,2-diol

HRID 42197
ノート
印刷プレビュー

反応式

HRID 42197 の反応式
[CH2:1]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([N:18]2[CH2:23][CH2:22][N:21]([C:24]3[CH:29]=[CH:28][C:27]([C:30]([CH3:32])=[CH2:31])=[CH:26][N:25]=3)[CH2:20][CH2:19]2)=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)=[O:35].C[N+]1([O-])CCOCC1.S([O-])([O-])=O.[Na+].[Na+].[OH2:51]>O.O.[O-][Os]([O-])(=O)=O.[K+].[K+].C(O)(C)(C)C>[CH2:1]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([N:18]2[CH2:19][CH2:20][N:21]([C:24]3[N:25]=[CH:26][C:27]([C:30]([OH:35])([CH3:32])[CH2:31][OH:51])=[CH:28][CH:29]=3)[CH2:22][CH2:23]2)=[N:10][N:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 180AcetoneHCID 962Water2 回HCID 24437Sodium SulfiteHCID 82029Methyl morpholine oxideHCID 44186377HCID 44186377、化合物

生成物 1

HCID 441863782-{6-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyridin-3-yl}-propane-1,2-diol収率 72%

試薬・触媒・溶媒 2

HCID 53393272Potassium osmate(VI) dihydrate触媒HCID 6386tert-Butanol溶媒

実験手順

To 1-benzyl-4-[4-(5-isopropenyl-pyridin-2-yl)-piperazin-1-yl]-phthalazine (68 mg, 0.158 mmol) is added acetone (1 mL), t-butanol (0.5 mL), and H2O (0.5 mL). To this suspension is then added potassium osmate (VI) dihydrate (536 μg, 1.58 μM), and NMO (21 mg, 0.174 mmol), and the reaction is stirred at room temperature for 3 h. Sodium sulfite (350 mg) is added to the resulting clear orange solution and the mixture is stirred for 1 h. Additional H2O (25 mL) is added, and the organics extracted with EtOAc (3×25 mL), dried over MgSO4, and concentrated. Purification by flash chromatography on silica gel (90:10 CH2Cl2:MeOH) afforded a clear oil which was then triturated with EtOAc to afford the title compound as a white powder (52 mg, 72% yield).

後処理

  1. extractionthe organics extracted with EtOAc (3×25 mL)
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated
  4. customPurification by flash chromatography on silica gel (90:10 CH2Cl2:MeOH)
  5. customafforded a clear oil which
  6. customwas then triturated with EtOAc

出典と根拠

ORDレコード
ord-009f8c573ce6455c8b254aa7822ef177
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08536168B2

反応ノート

読み込み中…

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