4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride → HCID 11283170, 화합물

HRID 751729노트

반응식

HRID 751729 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[CH:10]=[C:9]([C:11]([NH:13][C@@H:14]([CH2:18][C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)[C:15]([OH:17])=O)=[O:12])[NH:8][C:5]2=[CH:6][N:7]=1.C[N+]1(C2N=C(OC)N=C(OC)N=2)CCOCC1.[Cl-].[O:44]1[C:48]2([CH2:53][CH2:52][CH2:51][NH:50][CH2:49]2)[O:47][CH2:46][CH2:45]1>C(O)C>[O:44]1[C:48]2([CH2:53][CH2:52][CH2:51][N:50]([C:15](=[O:17])[C@@H:14]([NH:13][C:11]([C:9]3[NH:8][C:5]4=[CH:6][N:7]=[C:2]([Cl:1])[CH:3]=[C:4]4[CH:10]=3)=[O:12])[CH2:18][C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)[CH2:49]2)[O:47][CH2:46][CH2:45]1

참가 물질

5

반응물 3

HCID 27340594-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chlorideHCID 123947731,4-Dioxa-7-azaspiro[4.5]decaneHCID 597536992-(S)-[(5-Chloro-1H-pyrrolo[2,3-c]pyridine-2-carbonyl)amino]-3-(4-fluorophenyl)propionic acid

생성물 1

HCID 11283170HCID 11283170, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of 2-(S)-[(5-chloro-1H-pyrrolo[2,3-c]pyridine-2-carbonyl)amino]-3-(4-fluorophenyl)propionic acid (EXAMPLE 228, 80 mg, 0.22 mmol) in ethanol (6 mL) was added DMTMM (78 mg, 0.27 mmol) and the reaction stirred for 5 min. To the mixture was added 1,4-dioxa-7-aza-spiro[4.5]decane (Preparation 94, 35 mg, 0.24 mmol) and stirring continued for 16 h. Solvent was removed in vacuo and the crude material partitioned between ethyl acetate and water. The organic layer was washed with NaHCO3 solution (2×20 mL) then brine (2×20 mL), dried (MgSO4) and the solvent removed in vacuo. Purification by chromatography using dichloromethane/methanol (95:5) as the eluent gave the title compound as a pale yellow powder. m/z (ES+)=487.21 [M+H]+; RT=3.50 min.

후처리

  1. stirringstirring
  2. waitcontinued for 16 h
  3. customSolvent was removed in vacuo
  4. customthe crude material partitioned between ethyl acetate and water
  5. washThe organic layer was washed with NaHCO3 solution (2×20 mL)
  6. dry with materialbrine (2×20 mL), dried (MgSO4)
  7. customthe solvent removed in vacuo
  8. customPurification by chromatography

출처 및 근거

ORD 기록
ord-24c7b09752ea47bc91cc9e2bddc5ecfd
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405210B2

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