Hydrochloric Acid → HCID 3309686, 화합물

HRID 975184노트

반응식

HRID 975184 반응식
[CH3:1][C:2]([O:4][CH2:5][C:6]1[CH2:25][S:24][C@@H:9]2[C@H:10]([NH:13][C:14]([C@H:16]([NH2:23])[C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)=[O:15])[C:11](=[O:12])[N:8]2[C:7]=1[C:26]([OH:28])=[O:27])=[O:3].Cl>>[C:2]([O:4][CH2:5][C:6]1[CH2:25][S:24][CH:9]2[N:8]([C:11](=[O:12])[CH:10]2[NH:13][C:14](=[O:15])[CH:16]([NH2:23])[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:7]=1[C:26]([OH:28])=[O:27])(=[O:3])[CH3:1]

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 19150Cephaloglycin

생성물 1

HCID 3309686HCID 3309686, 화합물수율 84.2%

반응 조건

온도
25 °C

실험 절차

The resultant crude protected cephaloglycin mixture is worked up by treating with a mixture of 27 ml ice-water and 6 ml concentrated HCl and stirred for 15 minutes while cooling with ice. The aqueous phase is separted off and the organic phase is back-extracted with 2 ml ice-water. The combined aqueous phases are heated to 25° C. and TEA is added until a pH value of 4.5/4.7 is reached. The title compound is obtained in the dihydrate form by standing the mixture 30 minutes, filtering the crystals and washing then with 30 ml ice-water and 30 ml 80% acetone, followed by drying. Yield 84.2%.

후처리

  1. temperaturewhile cooling with ice
  2. extractionthe organic phase is back-extracted with 2 ml ice-water
  3. additionTEA is added until a pH value of 4.5/4.7

출처 및 근거

ORD 기록
ord-1298fe93693e4b5c89d9ff554c481daf
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05608055

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