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Bromotrimethylsilane → HCID 178502819, 화합물

HRID 894827
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HRID 894827 반응식
Br[Si](C)(C)C.C[O:7][P:8]([NH:12][C:13]([O:15][CH2:16][C:17]1[CH2:18][S:19][C@@H:20]2[C@H:33]([NH:34][C:35](=[O:45])/[C:36](/[C:40]3[O:41][CH:42]=[CH:43][CH:44]=3)=[N:37]\[O:38][CH3:39])[C:32](=[O:46])[N:21]2[C:22]=1[C:23]([O:25][CH:26]([O:28][C:29](=[O:31])[CH3:30])[CH3:27])=[O:24])=[O:14])([O:10]C)=[O:9].[CH3:47][Si](NC(OCC)=O)(C)C>ClCCl>[CH:42]([O:41][CH:40]([CH3:36])[CH3:44])([CH3:43])[CH3:47].[P:8]([NH:12][C:13]([O:15][CH2:16][C:17]1[CH2:18][S:19][C@@H:20]2[C@H:33]([NH:34][C:35](=[O:45])/[C:36](/[C:40]3[O:41][CH:42]=[CH:43][CH:44]=3)=[N:37]\[O:38][CH3:39])[C:32](=[O:46])[N:21]2[C:22]=1[C:23]([O:25][CH:26]([O:28][C:29](=[O:31])[CH3:30])[CH3:27])=[O:24])=[O:14])([OH:9])([OH:10])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 76113BromotrimethylsilaneHCID 11355656N-trimethylsilylurethaneHCID 178502818HCID 178502818, 화합물

생성물 2

HCID 7914Diisopropyl EtherHCID 178502819HCID 178502819, 화합물수율 133.8%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

Bromotrimethylsilane (0.31 g) in dichloromethane (3 ml) was added to a cooled (0°) stirred mixture of (R and S)-1-acetoxyethyl (6R,7R)-3-dimethoxyphosphorylcarbamoyloxymethyl-7-[Z-2-(fur-2-yl)-2-methoxyiminoacetamido]ceph-3-em-4-carboxylate (0.62 g) and trimethylsilylurethane (0.16 g) in dry dichloromethane (12 ml) in a nitrogen atmosphere. After 2.5 hours the reaction mixture was evaporated in vacuo to a foam. This foam was dissolved in ethyl acetate (30 ml) although a slight precipitate remained. The filtered organic solution was treated with saturated aqueous sodium bicarbonate solution (30 ml) and the aqueous solution was layered with butan-1-ol (20 ml) and acidified to pH 0.5 by addition of concentrated hydrochloric acid. The aqueous phase was extracted with butan-1-ol (2×15 ml) and the combined organic extracts were evaporated in vacuo to give a solid. Trituration of this solid with di-isopropyl ether afforded the title ester (0.396 g) as a solid; νmax (Nujol) 3270 (NH), 1788 (β-lactam), 1734 (CO2R) and 1684 and 1540 cm-1 (CONH); τ (DMSO-d6) 0.18 (d, J 8 Hz, NH), 2.9 to 3.4 (broad m, 2 superimposed q, CHCH3), 4.14 (m, 7-H, mixture of diastereoisomers), 4.76 (m, 6-H, mixture of diastereoisomers), 7.92 (s, OCOCH3) and 8.52 (d, J 5 Hz, CHCH3).

후처리

  1. temperaturea cooled (0°)
  2. customAfter 2.5 hours the reaction mixture was evaporated in vacuo to a foam
  3. dissolutionThis foam was dissolved in ethyl acetate (30 ml) although a slight precipitate
  4. additionThe filtered organic solution was treated with saturated aqueous sodium bicarbonate solution (30 ml)
  5. additionacidified to pH 0.5 by addition of concentrated hydrochloric acid
  6. extractionThe aqueous phase was extracted with butan-1-ol (2×15 ml)
  7. customthe combined organic extracts were evaporated in vacuo
  8. customto give a solid

출처 및 근거

ORD 기록
ord-19471d4147dd4292a9ec51c979856bb4
출처 데이터셋
uspto-grants-1981_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04284766

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