Methanesulfonic Acid → HCID 86584033, 화합물

HRID 427355노트

반응식

HRID 427355 반응식
[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

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 9846516AR-A000002

생성물 1

HCID 86584033HCID 86584033, 화합물수율 31%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

(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 C27H36N4O2×CH4O3S×2H2O: C, 57.9; H, 7.6; N, 9.7. Found: C, 58.1; H, 7.4; N, 9.6.

후처리

  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

출처 및 근거

ORD 기록
ord-82296297e0844d0eb0dba44a83291678
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313118B1

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