Hydrochloric Acid → 1-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]piperidin-4-amine

HRID 2353674노트

반응식

HRID 2353674 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]([N:19]2[CH2:24][CH2:23][CH:22]([NH:25]C(=O)OC(C)(C)C)[CH2:21][CH2:20]2)[N:9]=1.Cl.C(=O)(O)[O-].[Na+]>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:16])=[O:17])[N:11]=[C:10]([N:19]2[CH2:20][CH2:21][CH:22]([NH2:25])[CH2:23][CH2:24]2)[N:9]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 59380100tert-Butyl N-[1-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]-4-piperidyl]carbamate

생성물 1

HCID 593800761-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]piperidin-4-amine수율 102.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

tert-Butyl N-[1-[4-[(3S)-3-methylmorpholin-4-yl]-6-(methylsulfonylmethyl)pyrimidin-2-yl]-4-piperidyl]carbamate (1.30 g, 2.77 mmol) was dissolved in methanol (10 mL). 4M Hydrochloric acid in dioxane (10 mL) was added. The reaction was stirred at RT for 3 hours. Saturated aqueous sodium bicarbonate was added until pH7 was reached and the organic solvents were removed in vacuo. Water (20 mL) was added and the product was extracted into ethyl acetate (50 mL). The aqueous layer was extracted with a second portion of ethyl acetate (25 mL). The combined organics were evaporated to give the desired material as a yellow foam (1.05 g).

후처리

  1. customthe organic solvents were removed in vacuo
  2. additionWater (20 mL) was added
  3. extractionthe product was extracted into ethyl acetate (50 mL)
  4. extractionThe aqueous layer was extracted with a second portion of ethyl acetate (25 mL)
  5. customThe combined organics were evaporated

출처 및 근거

ORD 기록
ord-2f678d16e7dd49228156f15b755afa38
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07750003B2

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