홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Iodine → 3-(2-Aminothiazol-5-yl)-2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene

HRID 2413404
노트
인쇄 미리보기

반응식

HRID 2413404 반응식
II.[CH:3]([O:16][C:17]([C:19]1[N:20]2[CH:23]([S:24][CH2:25][C:26]=1[CH:27]=[CH:28]N(C)C)[CH:22]([NH:32][C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[C:21]2=[O:40])=[O:18])([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[NH2:41][C:42]([NH2:44])=[S:43]>C(Cl)Cl.O1CCCC1.O.C(OCC)(=O)C>[NH2:41][C:42]1[S:43][C:27]([C:26]2[CH2:25][S:24][CH:23]3[N:20]([C:21](=[O:40])[CH:22]3[NH:32][C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[C:19]=2[C:17]([O:16][CH:3]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[O:18])=[CH:28][N:44]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 807IodineHCID 2723790Thiourea2회HCID 539143342-Benzhydryloxycarbonyl-7-t-butoxycarbonylamino-3-(2-dimethylamino-vinyl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene

생성물 1

HCID 131759453-(2-Aminothiazol-5-yl)-2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene

시약·촉매·용매 4

HCID 962
Water
용매
2회
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매2회
HCID 8857Ethyl Acetate용매

실험 절차

A suspension of iodine (2.54 g) in dry methylene chloride (20 cc) is added, in 5 minutes, to a solution, cooled to -55° C., of 2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-3-(2-dimethylamino-vinyl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene, E-form (5.35 g) in dry tetrahydrofuran (20 cc). The reaction mixture is stirred for 2 hours, whilst allowing the temperature gradually to return to 0° C., and is then treated with distilled water (0.36 cc) and stirred for 2 hours at 5° C. A solution of thiourea (0.57 g) in a mixture of tetrahydrofuran (5 cc) and water (2 cc) is added to 25 cc of this reaction mixture and this mixture is stirred for 16 hours at 25° C. Thiourea (0.57 g) is added, stirring is continued for 3 hours at 25° C., and the mixture is then diluted with ethyl acetate (150 cc). The organic phase is washed successively with distilled water (100 cc), saturated sodium bicarbonate solution (100 cc), distilled water (100 cc) and a half-saturated sodium chloride solution (100 cc). After having dried the mixture over magnesium sulphate, the solvent is evaporated under reduced pressure (30 mm Hg; 4 kPa) at 30° C. The residue is chromatographed on a column (height: 30 cm; diameter: 2 cm) of silica (0.04-0.06 mm), elution being carried out under 0.4 bar (40 kPa) with a 45:55 (by volume) mixture of cyclohexane and ethyl acetate. After evaporation of the solvents, 3-(2-amino-thiazol-5-yl)-2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-8-oxo-5-thia-1-azabicyclo[4.2.0]-oct-2-ene (0.08 g) is obtained in the form of an orange froth, whose characteristics are identical to those of the product described below, in Example 2.

후처리

  1. additionis added, in 5 minutes, to a solution
  2. customto return to 0° C.
  3. stirringstirred for 2 hours at 5° C
  4. stirringthis mixture is stirred for 16 hours at 25° C
  5. stirringstirring
  6. waitis continued for 3 hours at 25° C.
  7. washThe organic phase is washed successively with distilled water (100 cc), saturated sodium bicarbonate solution (100 cc)
  8. distillationdistilled water (100 cc)
  9. dry with materialAfter having dried the mixture over magnesium sulphate
  10. customthe solvent is evaporated under reduced pressure (30 mm Hg; 4 kPa) at 30° C
  11. customThe residue is chromatographed on a column (height: 30 cm; diameter: 2 cm) of silica (0.04-0.06 mm), elution
  12. additionbeing carried out under 0.4 bar (40 kPa) with a 45:55 (by volume) mixture of cyclohexane and ethyl acetate
  13. customAfter evaporation of the solvents

출처 및 근거

ORD 기록
ord-575eaea066794a528834d19548d9901e
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04496560

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트