tert-Butyl N,N-dipropan-2-ylcarbamimidate → HCID 178450703, 화합물

HRID 839021노트

반응식

HRID 839021 반응식
[NH2:1][CH:2]1[C:25](=[O:26])[N:4]2[C:5]([C:22]([OH:24])=[O:23])=[C:6]([CH:9]([S:16][C:17]3[NH:21][N:20]=[N:19][N:18]=3)[CH2:10][CH2:11][S:12](=[O:15])(=[O:14])[NH2:13])[CH2:7][S:8][C@H:3]12.[C:27](OC(=N)N(C(C)C)C(C)C)([CH3:30])([CH3:29])[CH3:28]>C(Cl)Cl>[C:27]([O:23][C:22]([C:5]1[N:4]2[C:25](=[O:26])[CH:2]([NH2:1])[C@H:3]2[S:8][CH2:7][C:6]=1[CH:9]([S:16][C:17]1[NH:18][N:19]=[N:20][N:21]=1)[CH2:10][CH2:11][S:12](=[O:14])(=[O:15])[NH2:13])=[O:24])([CH3:30])([CH3:29])[CH3:28]

참가 물질

4

반응물 2

HCID 22010542tert-Butyl N,N-dipropan-2-ylcarbamimidateHCID 178508099HCID 178508099, 화합물

생성물 1

HCID 178450703HCID 178450703, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a suspension of 21.1 g (0.05 mol.) of 7-amino-3-[1-(2-sulfamoylethyl)tetrazol-5-ylthiomethyl]-3-cephem-4-carboxylic acid in 500 ml. of dry methylene chloride is added in one portion a solution of 30.0 g. (0.15 mol.) of O-t-butyldiisopropylpseudourea in 50 ml. of methylene chloride. The mixture is stirred at ambient temperature for 24 hours. The precipitate is removed by filtration and the filtrate evaporated to a residue which is taken up in 200 ml. of benzene and filtered again. The filtrate is extracted with three 100 ml. portions of cold 1N hydrochloric acid. The acidic aqueous extracts are layered with ethyl acetate and the pH adjusted to 7.5 with solid sodium bicarbonate. The organic layer is separated and the aqueous phase is extracted with two 150 ml. portions of ethyl acetate. The combined extracts are dried (MgSO4), filtered and evaporated to give 7-amino-3-[1-(2-sulfamoylethyl)tetrazol-5-ylthiomethyl]-3-cephem-4-carboxylic acid t-butyl ester.

후처리

  1. customThe precipitate is removed by filtration
  2. customthe filtrate evaporated to a residue which
  3. filtrationof benzene and filtered again
  4. extractionThe filtrate is extracted with three 100 ml
  5. customThe organic layer is separated
  6. extractionthe aqueous phase is extracted with two 150 ml
  7. dry with materialThe combined extracts are dried (MgSO4)
  8. filtrationfiltered
  9. customevaporated

출처 및 근거

ORD 기록
ord-45f418a430af4c4d84c146ea2d44ca33
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093723

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