Hydrochloric Acid → HCID 178480925、化合物

HRID 1852547ノート

反応式

HRID 1852547 の反応式
Cl.C(OC(=O)[NH:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([NH:15][C:16](=[O:25])[CH2:17][N:18]2[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]2)[CH2:11][CH2:10]1)(C)(C)C.CCOCC>CO>[NH2:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([NH:15][C:16](=[O:25])[CH2:17][N:18]2[CH2:19][CH2:20][N:21]([CH3:24])[CH2:22][CH2:23]2)[CH2:13][CH2:14]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 178480926HCID 178480926、化合物

生成物 1

HCID 178480925HCID 178480925、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

An aqueous solution of HCl (2 M, 15 mL) was added to a solution of trans-{4-[2-(4-methyl-piperazin-1-yl)-acetylamino]-cyclohexyl}-carbamic acid tert-butyl ester (199 mg, 0.56 mmol) in MeOH (15 mL) at RT, and the resulting mixture was stirred overnight. The reaction mixture was concentrated under reduced pressure to give a solid residue. Et2O was added to this material, and the resulting suspension was sonicated. The ether phase was decanted away, leaving a powdery brown solid which was purified by preparative TLC. The resulting oil was dissolved in the minimum quantity of MeOH, and Et2O was added. A solid precipitated; the liquid phase was decanted away to give, after drying, 75 mg of trans-N-(4-amino-cyclohexyl)-2-(4-methyl-piperazin-1-yl)-acetamide as a fine powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto give a solid residue
  3. customthe resulting suspension was sonicated
  4. customThe ether phase was decanted away
  5. customleaving a powdery brown solid which
  6. customwas purified by preparative TLC
  7. dissolutionThe resulting oil was dissolved in the minimum quantity of MeOH, and Et2O
  8. additionwas added
  9. customA solid precipitated
  10. customthe liquid phase was decanted away
  11. customto give
  12. customafter drying

出典と根拠

ORDレコード
ord-9447c1ba99b44f1c87d452cbae8b3f1d
出典データセット
uspto-grants-2015_02
特許番号
US08962622B2

反応ノート

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