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Hydrochloric Acid → 6-Methyl-2-(2-((pyridin-3-yloxy)methyl)piperazin-1-yl)benzo[d]oxazole hydrochloride

HRID 1487781
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HRID 1487781 반응식
[ClH:1].O1CCOCC1.OC(C(F)(F)F)=O.OC(C(F)(F)F)=O.[CH3:22][C:23]1[CH:52]=[CH:51][C:26]2[N:27]=[C:28]([N:30]3[CH2:35][CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][CH:31]3[CH2:43][O:44][C:45]3[CH:46]=[N:47][CH:48]=[CH:49][CH:50]=3)[O:29][C:25]=2[CH:24]=1>CO>[ClH:1].[CH3:22][C:23]1[CH:52]=[CH:51][C:26]2[N:27]=[C:28]([N:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH:31]3[CH2:43][O:44][C:45]3[CH:46]=[N:47][CH:48]=[CH:49][CH:50]=3)[O:29][C:25]=2[CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 131728871HCID 131728871, 화합물

생성물 1

HCID 667967596-Methyl-2-(2-((pyridin-3-yloxy)methyl)piperazin-1-yl)benzo[d]oxazole hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4 M HCl in 1,4-dioxane (6 mL, 24 mmol) was added to a solution of tert-butyl 4-(6-methylbenzo[d]oxazol-2-yl)-3-((pyridin-3-yloxy)methyl)piperazine-1-carboxylate di-TFA salt (91.1 mg, 0.140 mmol) in MeOH (1 mL). After 2 h, the reaction mixture was concentrated under reduced pressure and purified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient). The fractions containing the desired product were brought to pH 12 with 1 N NaOH, and brine (20 mL) was added. This was extracted with EtOAc (3 x). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure, yielding 33.0 mg of the free-base of the desired product. The material was dissolved in MeOH (1 mL) and 4 M HCl in 1,4-dioxane (0.025 mL) was added. The mixture was concentrated under reduced pressure to give 35.5 mg (70%) of the desired product as the hydrochloride salt. LC-MS: RT=4.40 min, [M+H]+=325.1.

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. custompurified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient)
  3. additionThe fractions containing the desired product
  4. additionwas added
  5. extractionThis was extracted with EtOAc (3 x)
  6. dry with materialThe combined organics were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2c0280ef2c5846d58f147a9de420780e
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428522B2

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