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Trifluoroacetic acid → (R)-1-chloro-4-(2-methylpiperazin-1-yl)phthalazine

HRID 1689951
ノート
印刷プレビュー

反応式

HRID 1689951 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([N:12]2[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][C@H:13]2[CH3:25])=[N:4][N:3]=1.FC(F)(F)C(O)=O.C([O-])(O)=O.[Na+]>ClCCl>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][C@H:13]2[CH3:25])=[N:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 57581470(R)-tert-butyl 4-(4-chlorophthalazin-1-yl)-3-methylpiperazine-1-carboxylate

生成物 1

HCID 57581473(R)-1-chloro-4-(2-methylpiperazin-1-yl)phthalazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(R)-tert-butyl 4-(4-chlorophthalazin-1-yl)-3-methylpiperazine-1-carboxylate (1.20 g, 3.31 mmol) was dissolved in dry dichloromethane (40 mL). Trifluoroacetic acid (8 mL) was added dropwise and allowed to stir at RT for 2 hours. The reaction was added to saturated NaHCO3 (200 mL) and the aqueous phase was extracted with 3×100 mL of dichloromethane. The combined organics were dried (MgSO4) and evaporated to give a pale yellow solid. MS (M+H)+=263.1.

後処理

  1. extractionthe aqueous phase was extracted with 3×100 mL of dichloromethane
  2. dry with materialThe combined organics were dried (MgSO4)
  3. customevaporated
  4. customto give a pale yellow solid

出典と根拠

ORDレコード
ord-288fdd5b4c6f4014a9ee7b41a6ea0281
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153633B2

反応ノート

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