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Carbamate → Trifluoroacetic acid

HRID 1891230
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HRID 1891230 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:11][CH:10]([C:12]2[CH:49]=[CH:48][C:15]([CH2:16][O:17][C:18]3[C:23]([C:24]([F:27])([F:26])[F:25])=[CH:22][CH:21]=[CH:20][C:19]=3[C:28]3[N:33]=[C:32]([N:34]4[C:38]([C:39]([F:42])([F:41])[F:40])=[C:37]([C:43]([O:45]CC)=[O:44])[CH:36]=[N:35]4)[CH:31]=[CH:30][CH:29]=3)=[CH:14][CH:13]=2)[CH2:9]1)=[O:7])(C)(C)C.[C:50]([OH:56])([C:52]([F:55])([F:54])[F:53])=[O:51].CCN(C(C)C)C(C)C.ClC(OC)=O.C(=O)([O-])N.[OH-].[Li+].Cl>C(Cl)Cl.O1CCOCC1.C(#N)C>[C:50]([OH:56])([C:52]([F:55])([F:54])[F:53])=[O:51].[CH3:1][O:5][C:6]([N:8]1[CH2:9][CH:10]([C:12]2[CH:13]=[CH:14][C:15]([CH2:16][O:17][C:18]3[C:23]([C:24]([F:25])([F:26])[F:27])=[CH:22][CH:21]=[CH:20][C:19]=3[C:28]3[N:33]=[C:32]([N:34]4[C:38]([C:39]([F:41])([F:42])[F:40])=[C:37]([C:43]([OH:45])=[O:44])[CH:36]=[N:35]4)[CH:31]=[CH:30][CH:29]=3)=[CH:48][CH:49]=2)[CH2:11]1)=[O:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 7

HCID 276CarbamateHCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 6422Trifluoroacetic acid2회HCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 86644580HCID 86644580, 화합물

생성물 2

HCID 6422Trifluoroacetic acidHCID 46897231HCID 46897231, 화합물

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매2회HCID 312751,4-Dioxane용매

반응 조건

온도
50 °C

실험 절차

To a solution of the title compound from Example 148 Step C (170 mg, 0.246 mmol) in DCM (3 mL) was added TFA (1 mL). After 3 min, the reaction mixture was concentrated in vacuo to provide the crude TFA-salt, which was used without further purification: LCMS m/z 590.9 [M+1-1]+. A portion of the unpurified TFA salt (0.08 mmol) was dissolved in DCM (1 mL), and DIEA (130 μL, 0.74 mmol) was added, followed by methyl chloroformate (19 μL, 0.25 mmol). After 20 min, the reaction mixture was quenched by addition of sat aq NaHCO3 and the aqueous phase was extracted with DCM. The organic phase was separated and concentrated in vacuo to provide the unpurified carbamate, which was used without further purification: LCMS m/z 648.9 [M+H]+. To a solution of the carbamate in dioxane (2 mL) was added lithium hydroxide (1 mL, 2N aqueous, 2 mmol), and the mixture was stirred at 50° C. for 1 h, then at ambient temperature. After 15 h, the reaction mixture was rendered acidic by addition of HCl (2N aqueous), then was diluted with acetonitrile and purified by reverse phase HPLC (30 to 100% acetonitrile/water, both 0.1% v/v TFA) to provide the title compound: LCMS m/z 620.9 [M+H]+; 1H NMR (500 MHz, d6-DMSO) δ 8.34 (s, 1H), 8.22 (t, J=8.0 Hz, 1H), 8.07 (d, J=8.0 Hz, 1H), 7.95 (d, J=8.0 Hz, 1H), 7.88-7.86 (m, 2H), 7.54 (t, J=8.0 Hz, 1H), 7.32 (d, J=8.0 Hz, 2H), 7.13 (d, J=8.0 Hz, 2H), 4.54 (s, 2H), 4.33-4.26 (m, 2H), 3.90-3.81 (m, 3H), 3.59 (s, 3H).

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customto provide the crude TFA-salt, which
  3. customwas used without further purification
  4. waitAfter 20 min
  5. customthe reaction mixture was quenched by addition of sat aq NaHCO3
  6. extractionthe aqueous phase was extracted with DCM
  7. customThe organic phase was separated
  8. concentrationconcentrated in vacuo
  9. customto provide the unpurified carbamate, which
  10. customwas used without further purification
  11. customat ambient temperature
  12. waitAfter 15 h
  13. custompurified by reverse phase HPLC (30 to 100% acetonitrile/water

출처 및 근거

ORD 기록
ord-e61c1d494475409f8bf2c68f7b6072a0
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507512B2

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