Hydrochloric Acid → HCID 69936700, 화합물

HRID 1623860

반응식

HRID 1623860 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][C:10]2[CH:19]=[CH:18][C:17]([C:20]([N:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)=[O:21])=[CH:16][C:11]=2[C:12](OC)=[O:13])=[CH:4][CH:3]=1.[OH-].[Li+].Cl.C(N(C(C)C)CC)(C)C.[F:40][C:41]1[C:46]([NH2:47])=[CH:45][CH:44]=[CH:43][N:42]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>O1CCCC1.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][C:10]2[CH:19]=[CH:18][C:17]([C:20]([N:22]3[CH2:23][CH2:24][O:25][CH2:26][CH2:27]3)=[O:21])=[CH:16][C:11]=2[C:12]([NH:47][C:46]2[C:41]([F:40])=[N:42][CH:43]=[CH:44][CH:45]=2)=[O:13])=[CH:4][CH:3]=1

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 81531DiisopropylethylamineHCID 27628162-Fluoropyridin-3-amineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 67106885HCID 67106885, 화합물

생성물 1

HCID 69936700HCID 69936700, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

To a solution of methyl 2-{[(4-fluorophenyl)methyl]oxy}-5-(4-morpholinylcarbonyl)benzoate (may be prepared as described in Description 109, 93 mg, 0.25 mmol) in tetrahydrofuran (4 ml) was added lithium hydroxide (19 mg, 0.79 mmol) and water (1 ml). The mixture was stirred at 50° C. for one hour, cooled and 2M hydrochloric acid (0.40 ml, 0.80 mmol) was added and the solvent removed in vacuo The residue was redissolved in N,N-dimethylformamide (4 ml) and diisopropylethylamine (0.11 ml, 0.62 mmol), 2-fluoro-3-pyridinamine (36.3 mg, 0.32 mmol) and HATU (284 mg, 0.75 mmol) were added. The solvent was removed in vacuo and the residue purified by MDAP to yield the title compound as an off-white solid. 5 mg.

후처리

  1. temperaturecooled
  2. customthe solvent removed in vacuo The residue
  3. dissolutionwas redissolved in N,N-dimethylformamide (4 ml)
  4. customThe solvent was removed in vacuo
  5. customthe residue purified by MDAP

출처 및 근거

ORD 기록
ord-5939f64444684457a3094a7c83317634
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08778939B2

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