Trifluoroacetic acid → HCID 22288423、化合物

HRID 968246ノート

反応式

HRID 968246 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][C:11]2[CH:12]=[C:13]([NH:18]C(=O)OC(C)(C)C)[CH:14]=[C:15]([CH3:17])[CH:16]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][C:11]2[CH:12]=[C:13]([CH:14]=[C:15]([CH3:17])[CH:16]=2)[NH2:18])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22288425Tert-butyl 3-[(4-acetylpiperazin-1-yl)methyl]-5-methylphenylcarbamate

生成物 1

HCID 22288423HCID 22288423、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 3-[(4-acetylpiperazin-1-yl)methyl]-5-methylphenylcarbamate (306 mg, 0.88 mmol) in CH2Cl2 (4 mL) was added TFA (4 mL) at room temperature. After 2 hours the mixture was concentrated. The residue was taken up in saturated NaHCO3 and extracted with CH2Cl2 (3×). The combined organic layers were dried (MgSO4), filtered, and concentrated to give 3-[(4-acetylpiperazin-1-yl)methyl]-5-methylaniline as a white solid. 1H-NMR (300 MHz, CDCl3) δ 6.52 (s, 1H), 6.48 (s, 1H), 6.43 (s, 1H), 3.62 (m, 4H), 3.45 (m, 2H), 3.39 (s, 2H), 2.40 (m, 4H), 2.25 (s, 3H), 2.08 (s, 3H).

後処理

  1. concentrationAfter 2 hours the mixture was concentrated
  2. extractionextracted with CH2Cl2 (3×)
  3. dry with materialThe combined organic layers were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-20bf7ca4cfab45a5ab8a254c9f417a02
出典データセット
uspto-grants-2005_10
特許番号
US06958340B2

反応ノート

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