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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ammonia → HCID 20560975, 화합물

HRID 1155500
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HRID 1155500 반응식
[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][C:11](=O)[CH2:10][CH2:9]2)[CH:5]=[N:4][CH:3]=1.N.[BH3-]C#[N:18].[Na+].Cl>CO>[ClH:1].[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][CH:11]([NH2:18])[CH2:10][CH2:9]2)[CH:5]=[N:4][CH:3]=1
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참가 물질

6

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HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 5003444Sodium cyanoborohydrideHCID 128022151-(6-Chloropyrazin-2-yl)piperidin-4-one

생성물 1

HCID 20560975HCID 20560975, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 17.1 g (81 mmol) 6-chloro-2-(4-oxopiperidino)pyrazine in 250 ml methanol which has been saturated with gaseous NH3 is added 62.4 g (0.81 mol) NH4OAc and 5.0 g (80 mmol) NaCNBH3. After stirring at 20°-25° C. for 60 hours, the MeOH is removed in vacuo. Water is added to the residue, and the pH is adjusted to 14. The product is extracted into ethyl acetate which is dried and concentrated. Chromatography of the residue over silica gel, eluting with 5% MeOH/CHCl3 saturated with NH3, gives the product base which is converted to the hydrochloride salt with ethanolic HCl. Recrystallization from water/acetone affords the desired product, m.p. 291° C. (dec.).

후처리

  1. customthe MeOH is removed in vacuo
  2. additionWater is added to the residue
  3. extractionThe product is extracted into ethyl acetate which
  4. customis dried
  5. concentrationconcentrated
  6. washChromatography of the residue over silica gel, eluting with 5% MeOH/CHCl3 saturated with NH3
  7. customgives the product base which
  8. customRecrystallization from water/acetone

출처 및 근거

ORD 기록
ord-fafb320e31184145af10aa444e9c7dd2
출처 데이터셋
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04302455

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