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Hydrochloric Acid → HCID 10391157, 화합물

HRID 736463
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HRID 736463 반응식
C([Li])CCC.B(OC(C)C)(OC(C)C)OC(C)C.Br[C:20]1[CH:25]=[CH:24][C:23]([S:26]([N:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)(=[O:28])=[O:27])=[CH:22][CH:21]=1.[ClH:34].C(=O)([O-])[O-].[Na+].[Na+].[NH2:41][C:42]1[C:43]([C:49]([NH:51][CH2:52][CH2:53][N:54]2[CH2:59][CH2:58][O:57][CH2:56][CH2:55]2)=[O:50])=[N:44][C:45](Br)=[CH:46][N:47]=1>O1CCCC1.CO.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[ClH:34].[NH2:41][C:42]1[C:43]([C:49]([NH:51][CH2:52][CH2:53][N:54]2[CH2:59][CH2:58][O:57][CH2:56][CH2:55]2)=[O:50])=[N:44][C:45]([C:20]2[CH:25]=[CH:24][C:23]([S:26]([N:29]3[CH2:33][CH2:32][CH2:31][CH2:30]3)(=[O:28])=[O:27])=[CH:22][CH:21]=2)=[CH:46][N:47]=1
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참가 물질

10

반응물 6

HCID 313Hydrochloric Acid2회HCID 10340Sodium CarbonateHCID 21531Triisopropyl borateHCID 7386181-(4-Bromobenzene-1-sulfonyl)pyrrolidineHCID 10426742HCID 10426742, 화합물HCID 178418339Butyllithium

생성물 1

HCID 10391157
HCID 10391157, 화합물
수율 26%

시약·촉매·용매 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

n-Butyllithium (1.6 mL, 2.6 mmol) was added dropwise over 10 min to a cooled solution (−78° C.) of triisopropyl borate (0.6 mL, 2.6 mmol), and 1-[(4-bromophenyl)sulfonyl]pyrrolidine (0.251 g, 0.86 mmol) in anhydrous tetrahydrofuran (10 mL) under an atmosphere of nitrogen. The resulting mixture was stirred at −78° C. for 1 h and the mixture was allowed to warm up to room temperature. Aqueous HCl (3 M, 1.4 mL, 4.3 mmol) was added and the mixture was stirred for 10 min followed by the addition of sodium carbonate (0.9 g, 8.6 mmol) and the stirring was continued for another 20 min. 3-Amino-6-bromo-N-(2-morpholin-4-ylethyl)pyrazine-2-carboxamide (0.20 g, 0.61 mmol), and tetrahydrofuran (4 mL) were added followed by addition of Pd(dppf)Cl2 (28 mg, 0.03 mmol) and the resulting mixture was heated at 65° C. for 17 h. The mixture was allowed to return to room temperature and the solvent was evaporated. The resulting residue was suspended in methanol, silica was added, and the solvent was evaporated. Purification by column chromatography on silica using methylene chloride/methanol/triethyl amine, (95:5:0.1), as the eluent gave the free base that was subsequently dissolved in hot methanol and treated with HCl (1 M in diethyl ether). The formed precipitate was filtered off and dried in vacuo to give 72 mg (26% yield) of the title compound as a yellow solid: 1H NMR (DMSO-d6, 400 MHz) δ 11.24 (br s, 1H), 9.28 (m, 1H), 8.98 (s, 1H), 8.49 (d, J=8 Hz, 2H), 7.83 (d, J=8 Hz, 2H), 3.97 (m, 2H), 3.87 (d, J=12 Hz, 2H), 3.78 (m, 2H), 3.55 (d, J=12 Hz, 2H), 3.15 (m, 6H), 1.65 (m, 4H); MS (ES) m/z 461 (M++1).

후처리

  1. temperatureto warm up to room temperature
  2. stirringthe mixture was stirred for 10 min
  3. waitthe stirring was continued for another 20 min
  4. temperaturethe resulting mixture was heated at 65° C. for 17 h
  5. customto return to room temperature
  6. customthe solvent was evaporated
  7. additionsilica was added
  8. customthe solvent was evaporated
  9. customPurification by column chromatography on silica
  10. customgave the free base that
  11. filtrationThe formed precipitate was filtered off
  12. customdried in vacuo

출처 및 근거

ORD 기록
ord-f909d4eeb4db48aea4ba57f3131c9267
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07595321B2

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