Morpholine-4-carboximidamide Hydrobromide → HCID 178418872, 화합물

HRID 8606

반응식

HRID 8606 반응식
CO[C:3](=[O:18])[CH:4]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[CH:11]=1)[C:5]([O:7]C)=O.C[O-].[Na+].Br.[N:23]1([C:29]([NH2:31])=[NH:30])[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>CO>[CH3:17][O:16][C:12]1[CH:11]=[C:10]([CH:15]=[CH:14][CH:13]=1)[O:9][C:4]1[C:3]([OH:18])=[N:30][C:29]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)=[N:31][C:5]=1[OH:7]

참가 물질

5

반응물 3

HCID 2806564Morpholine-4-carboximidamide HydrobromideHCID 10942334Sodium MethoxideHCID 21803851Dimethyl-(3-methoxyphenoxy)malonate

생성물 1

HCID 178418872HCID 178418872, 화합물수율 75.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of dimethyl-(3-methoxyphenoxy)-malonate (11.19 g) in methanol (100 ml) was added sodium methylate (6.48 g). The yellow solution was stirred for 6 h at rt. Then, morpholine-4-carboxamidine hydrobromide (8.40 g) was added and the mixture was stirred at rt for 16 h. The solvent was removed in vacuo and the residue was dissolved in water (150 ml) and extracted twice with diethyl ether (150 ml). The aqueous phase was acidified with 10% aq. citric acid. The solid that separated was collected, washed with water, evaporated twice from EA, and dried under high vacuum to give 5-(3-methoxy-phenoxy)-2-morpholin-4-yl-pyrimidine-4,6-diol (9.66 g) as a beige powder. LC-MS: tR=2.88 min, [M+1]+=320.19, [M−1]−=318.02.

후처리

  1. stirringthe mixture was stirred at rt for 16 h
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in water (150 ml)
  4. extractionextracted twice with diethyl ether (150 ml)
  5. customThe solid that separated
  6. customwas collected
  7. washwashed with water
  8. customevaporated twice from EA
  9. customdried under high vacuum

출처 및 근거

ORD 기록
ord-c7258cdcfc7c44909a8bab2d91687812
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091201B2

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