Methanesulfonic Acid → HCID 86584033、化合物

HRID 1862063ノート

反応式

HRID 1862063 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[C:8]2[C:3]=1[CH2:4][CH2:5][C@@H:6]([NH:19][C:20](=[O:33])[C:21]1[CH:26]=[CH:25][C:24]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)=[CH:23][CH:22]=1)[CH2:7]2.[CH3:34][S:35]([OH:38])(=[O:37])=[O:36]>O1CCCC1>[CH3:34][S:35]([OH:38])(=[O:37])=[O:36].[CH3:1][C:2]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[C:8]2[C:3]=1[CH2:4][CH2:5][C@@H:6]([NH:19][C:20](=[O:33])[C:21]1[CH:26]=[CH:25][C:24]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)=[CH:23][CH:22]=1)[CH2:7]2

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 9846516AR-A000002

生成物 1

HCID 86584033HCID 86584033、化合物収率 31%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

(R)-N-[5-Methyl-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydro-2-naphthyl]-4-morpholinobenzamide (100 mg, 0.22 mmol) was dissolved in tetrahydrofuran (15 mL) and methanesulfonic acid (42 mg, 0.44 mmol), dissolved in tetrahydrofuran (5 mL), was added dropwise. The solvent was removed in vacuo to give a white solid that was recrystallized from acetone (5 mL) and then from a 15% H2O in acetone solution (7 mL). The crystals were filtered to give 37 mg (31% yield) of light yellow crystals that was stored in an exicator over blue gel: mp 250° C. (decom.). Anal. Calcd. for C27H36N4O2xCH40Sx2H2O: C, 57.9; H, 7.6; N, 9.7. Found: C, 58.1; H, 7.4; N, 9.6.

後処理

  1. additionwas added dropwise
  2. customThe solvent was removed in vacuo
  3. customto give a white solid
  4. customthat was recrystallized from acetone (5 mL)
  5. filtrationThe crystals were filtered
  6. customto give 37 mg (31% yield) of light yellow crystals that

出典と根拠

ORDレコード
ord-dd391cbdf86b4fb2a8186db1d5a4ba81
出典データセット
uspto-grants-2003_03
特許番号
US06534652B2

反応ノート

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