Hydrochloric Acid → 6-Acetyl-3-amino-pyrazine-2-carboxylic acid methyl ester

HRID 2368224노트

반응식

HRID 2368224 반응식
[CH3:1][O:2][C:3]([C:5]1[C:10]([NH:11]C(OC(C)(C)C)=O)=[N:9][CH:8]=[C:7]([C:19](=[O:21])[CH3:20])[N:6]=1)=[O:4].Cl>O1CCOCC1>[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][CH:8]=[C:7]([C:19](=[O:21])[CH3:20])[N:6]=1)=[O:4]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 700980376-Acetyl-3-tert-butoxycarbonylamino-pyrazine-2-carboxylic acid methyl ester

생성물 1

HCID 700984236-Acetyl-3-amino-pyrazine-2-carboxylic acid methyl ester수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a stirred solution of 6-acetyl-3-tert-butoxycarbonylamino-pyrazine-2-carboxylic acid methyl ester (500 mg, 1.69 mmol) at rt in dioxane (10 ml) under an argon atmosphere was added 4 M HCl solution in dioxane (4.23 ml, 16.9 mmol) in one portion. The reaction mixture was stirred overnight, then concentrated. The residue was triturated with Et2O, filtrated and dried. The solid was taken up in EtOAc (50 ml) and washed with saturated aqueous Na2CO3 solution (20 ml) and brine. The organic phase was dried over MgSO4, filtrated and concentrated to give the title compound (313 mg, 95%) as orange powder.

후처리

  1. concentrationconcentrated
  2. customThe residue was triturated with Et2O
  3. filtrationfiltrated
  4. customdried
  5. washwashed with saturated aqueous Na2CO3 solution (20 ml) and brine
  6. dry with materialThe organic phase was dried over MgSO4
  7. filtrationfiltrated
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e082f5f7c96d4811a38bea353405c02c
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703768B2

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