Acetic Acid → HCID 178451657, 화합물

HRID 1713111노트

반응식

HRID 1713111 반응식
C[O-].[Na+].[CH:4]([NH2:6])=[NH:5].O=[C:8]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10][CH:9]1[C:22](OC)=[O:23].C(O)(=O)C>CO>[OH:23][C:22]1[C:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:13][CH2:14][C:8]=2[N:6]=[CH:4][N:5]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 68047FormamidineHCID 10942334Sodium MethoxideHCID 57479414HCID 57479414, 화합물

생성물 1

HCID 178451657HCID 178451657, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of NaOMe in MeOH (13.6 mL, 25% in MeOH, 59.5 mmol) is added to a stirred solution of formamidine (2.2 g, 21 mmol) in MeOH (50 ml) at rt. The mixture is stirred for 15 min. 1-tert-Butyl 4-methyl 5-oxoazepane-1,4-dicarboxylate (5 g, 7.5 mmol) is added and the mixture is stirred at rt overnight. Acetic acid (2.33 g, 38.5 mmol) is added and the solvent is removed in vacuo. Water (30 ml) is added to the residue and the solution is extracted with DCM (3×30 ml). The combined extracts are washed with brine (40 ml), dried (Na2SO4) and evaporated, to provide a yellow solid that is used in the next step without further purification.

후처리

  1. stirringthe mixture is stirred at rt overnight
  2. customthe solvent is removed in vacuo
  3. additionWater (30 ml) is added to the residue
  4. extractionthe solution is extracted with DCM (3×30 ml)
  5. washThe combined extracts are washed with brine (40 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated
  8. customto provide a yellow solid that
  9. customis used in the next step without further purification

출처 및 근거

ORD 기록
ord-bbf2991210f548aa9c16d95d154514df
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795262B2

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