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Sodium Bicarbonate → HCID 21192697, 화합물

HRID 1418395
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HRID 1418395 반응식
O=[C:2]1[CH2:5][N:4]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:3]1.Cl.Cl.[NH2:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:15]=1[C:16]([NH2:18])=[NH:17].C(=O)(O)[O-].[Na+]>CN(C=O)C>[NH2:18][C:16]1[C:15]2[C:14](=[CH:22][CH:21]=[CH:20][C:19]=2[F:23])[NH:13][C:2]2([CH2:5][N:4]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:3]2)[N:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 4595261HCID 4595261, 화합물HCID 22008823HCID 22008823, 화합물

생성물 1

HCID 21192697HCID 21192697, 화합물수율 38.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Ethyl 3-oxoazetidine-1-carboxylate (Y. Nitta, T. Yamagouchi, T. Tanaka; Heterocycles, 1986, 24, 25) (175 mg, 1.22 mmol) and 2-amino-6-fluorobenzamidine dihydrochloride (Example C, 280 mg, 1.22 mmol) in dry DMF (10 ml) were heated at 80° C. for 4 hours. The resulting solution was cooled and poured into aqueous sodium bicarbonate solution and the resulting mixture was extracted with ethyl acetate. The extracts were concentrated and the residue purified by flash chromatography on silica eluting with dichloromethane/methanol (10:1) to give the title compound as a solid (0.13 g) m.p. 210°-212° C.

후처리

  1. temperatureThe resulting solution was cooled
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. concentrationThe extracts were concentrated
  4. customthe residue purified by flash chromatography on silica eluting with dichloromethane/methanol (10:1)

출처 및 근거

ORD 기록
ord-82a093017dbf43259db028bfbe524804
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05883102

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