Hydrochloric Acid → 4-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]aniline

HRID 1095407노트

반응식

HRID 1095407 반응식
[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[CH:13]=[C:12]([CH2:14][S:15]([CH3:18])(=[O:17])=[O:16])[N:11]=[C:10]([C:19]2[CH:24]=[CH:23][C:22]([NH:25]C(=O)OC(C)(C)C)=[CH:21][CH:20]=2)[N:9]=1.Cl>CO.O1CCOCC1>[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[CH:13]=[C:12]([CH2:14][S:15]([CH3:18])(=[O:17])=[O:16])[N:11]=[C:10]([C:19]2[CH:24]=[CH:23][C:22]([NH2:25])=[CH:21][CH:20]=2)[N:9]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 59508397tert-butyl N-[4-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]phenyl]carbamate

생성물 1

HCID 595083934-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]aniline

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

tert-Butyl N-[4-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]phenyl]carbamate (1.09 g, 2.35 mmol) was dissolved in methanol (5 mL) and 4M hydrogenchloride in dioxane (5 mL) was added. The solution was stirred at room temperature overnight, then the mixture evaporated to a dark brown oil and dissolved in ethyl acetate (10 mL). Water (5 mL) was added followed by the addition of sodium bicarbonate solution until neutral pH was achieved (˜2 mL). The phases were separated and the organic phase washed with water (10 mL). The organic layer was dried over magnesium sulphate and evaporated to a pale yellow foam (805 mg).

후처리

  1. customthe mixture evaporated to a dark brown oil
  2. dissolutiondissolved in ethyl acetate (10 mL)
  3. additionWater (5 mL) was added
  4. additionfollowed by the addition of sodium bicarbonate solution until neutral pH
  5. customThe phases were separated
  6. washthe organic phase washed with water (10 mL)
  7. dry with materialThe organic layer was dried over magnesium sulphate
  8. customevaporated to a pale yellow foam (805 mg)

출처 및 근거

ORD 기록
ord-ed4c7e6fb64549d6881af51a6ce0dec1
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138183B2

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