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

HRID 1095407ノート

反応式

HRID 1095407 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ed4c7e6fb64549d6881af51a6ce0dec1
出典データセット
uspto-grants-2012_03
特許番号
US08138183B2

反応ノート

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