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Methyl Carbamate → HCID 66549081, 화합물

HRID 2404391
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HRID 2404391 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:8]1[CH2:12][CH2:11][CH:10]([NH2:13])[CH2:9]1.C(N(CC)C(C)C)(C)C.O=C1CCC(=O)N1[O:30][C:31]([NH:33][C:34]1[CH:42]=[CH:41][CH:40]=[C:39]2[C:35]=1[CH:36]=[N:37][N:38]2C(OC)=O)=[O:32].C(=O)(OC)N.[OH-].[Na+]>O.CO.CN(C=O)C>[C:31](=[O:32])=[O:30].[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:8]1[CH2:12][CH2:11][C@@H:10]([NH:13][C:31]([NH:33][C:34]2[CH:42]=[CH:41][CH:40]=[C:39]3[C:35]=2[CH:36]=[N:37][NH:38]3)=[O:30])[CH2:9]1
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참가 물질

10

반응물 5

HCID 11722Methyl CarbamateHCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 11313556methyl 4-({[(2,5-dioxo-1-pyrrolidinyl)oxy]carbonyl}amino)-1H-indazole-1-carboxylateHCID 68313587HCID 68313587, 화합물

생성물 2

HCID 280Carbon Dioxide
HCID 66549081
HCID 66549081, 화합물
수율 91.8%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of Example 61B (0.35 g, 1.95 mmol), DMF (10 mL), N,N-diisopropyl ethylamine (0.72 mL, 4.1 mmol) and methyl 4-((2,5-dioxopyrrolidin-1-yloxy)carbonylamino)-1H-indazole-1-carboxylate (prepared as in Org. Proc. Res. Dev., 2007, 11, 578; 0.65 g, 1.95 mmol) was stirred at ambient temperature. After 5 minutes, LCMS showed complete conversion to the methyl carbamate intermediate. Methanol (20 mL) and 2N sodium hydroxide (5.86 mmol) were added resulting in a white slurry. The mixture was diluted with water and extracted with ethyl acetate (100 mL). The organic extract was washed with brine (50 mL), dried (Na2SO4), filtered and concentrated. The mixture was separated using a Chiralpak AD-H column and eluting with 5-50% MeOH:CO2 10 min at 3 mL/min to provide the title compound (303 mg, 31%) and Example 62 (181 mg, 27%). Data for Example 61C: 1H NMR (300 MHz, DMSO-d6) δ 12.98 (bs, 1H), 8.56 (s, 1H), 8.07 (d, J=1.0 Hz, 1H), 7.62 (d, J=7.9 Hz, 1H), 7.46-7.36 (m, 1H), 7.32-7.01 (m, 5H), 6.55 (d, J=7.2 Hz, 1H), 4.23-3.99 (m, 3H), 2.16-1.97 (m, 2H), 1.82-1.46 (m, 3H). MS (ESI+) M/Z 339 (M+H)+.

후처리

  1. customresulting in a white slurry
  2. extractionextracted with ethyl acetate (100 mL)
  3. extractionThe organic extract
  4. washwas washed with brine (50 mL)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe mixture was separated
  9. washeluting with 5-50% MeOH

출처 및 근거

ORD 기록
ord-ada8c79a21ae455c82154d7d1e22294d
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08802711B2

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