Ammonia → HCID 12942034, 화합물

HRID 543538

반응식

HRID 543538 반응식
COC(C1C(Cl)=C(Cl)C(C(OC)=O)=C(Cl)C=1Cl)=O.[SH:19][C:20]1[S:24][C:23]([CH3:25])=[N:22][N:21]=1.CC(O[CH2:30][C:31]1[CH2:40][S:39][C@@H:34]2[C@H:35]([NH2:38])[C:36](=[O:37])[N:33]2[C:32]=1[C:41]([OH:43])=[O:42])=O.N>C(#N)C>[NH2:38][CH:35]1[C:36](=[O:37])[N:33]2[C:32]([C:41]([OH:43])=[O:42])=[C:31]([CH2:30][S:19][C:20]3[S:24][C:23]([CH3:25])=[N:22][N:21]=3)[CH2:40][S:39][C@H:34]12

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 2943DacthalHCID 4413287-Aminocephalosporanic acidHCID 178434161HCID 178434161, 화합물

생성물 1

HCID 12942034HCID 12942034, 화합물수율 69.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A 14.8 g quantity of DCPA was cooled at 14° C., and 1.59 g of 5-mercapto-2-methyl-1,3,4-thiadiazole was added to it, whereby the mixture reached at the temperature of 25° C. and dissolved. 6.0 ml of acetonitrile was added and the solution was cooled at 15° C., to which 2.72 g of 7-ACA and 10.0 ml of acetonitrile were added, followed by stirring at 25° to 27° C. for 30 minutes. The reaction solution was poured into 80 g of ice-water, which was placed in a refrigerator overnight, adjusted to pH 4.0 with 25% aqueous ammonia and stirred for 1.0 hour under ice-cooling. The resultant precipitate was recovered by filtration, washed with 50 ml each of cold water and acetone successively, and dried, thereby affording 2.40 g of 7-amino-3-[(2-methyl-1,3,4-thiadiazol-5-yl)thiomethyl]-3-cephem-4-carboxylic acid.

후처리

  1. customreached at the temperature of 25° C.
  2. dissolutiondissolved
  3. additionwere added
  4. customwas placed in a refrigerator overnight
  5. stirringstirred for 1.0 hour under ice-
  6. temperaturecooling
  7. filtrationThe resultant precipitate was recovered by filtration
  8. washwashed with 50 ml each of cold water and acetone successively
  9. customdried

출처 및 근거

ORD 기록
ord-1976cbefe65a4a03a4083b0069489d98
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04446318

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