Lithium Carbonate → HCID 178451342, 화합물

HRID 1790591노트

반응식

HRID 1790591 반응식
C(=O)([O-])[O-].[Li+].[Li+].[C:7]([O:11][C:12]([CH2:14][O:15][C:16]1[C:21]([Cl:22])=[CH:20][C:19]([Cl:23])=[CH:18][C:17]=1[CH:24]([NH:29][C:30]1[CH:35]=[CH:34][C:33]([C:36](=[NH:39])[NH:37][OH:38])=[CH:32][CH:31]=1)[C:25]([O:27]C)=[O:26])=[O:13])([CH3:10])([CH3:9])[CH3:8]>C1COCC1.O>[C:7]([O:11][C:12]([CH2:14][O:15][C:16]1[C:21]([Cl:22])=[CH:20][C:19]([Cl:23])=[CH:18][C:17]=1[CH:24]([NH:29][C:30]1[CH:31]=[CH:32][C:33]([C:36](=[NH:39])[NH:37][OH:38])=[CH:34][CH:35]=1)[C:25]([OH:27])=[O:26])=[O:13])([CH3:10])([CH3:8])[CH3:9]

참가 물질

5

반응물 2

HCID 11125Lithium CarbonateHCID 178501559HCID 178501559, 화합물

생성물 1

HCID 178451342HCID 178451342, 화합물수율 83.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

3.7 g of finely powdered lithium carbonate were added to a solution of 1.96 g of methyl (RS)-(2-tert-butoxycarbonylmethoxy-3,5-dichloro-phenyl)-[4-(N-hydroxycarbamimidoyl)-phenylamino]-acetate (see Example 276.2) in 200 ml of THF and 100 ml of water. The suspension was stirred for 8 hours at 55–60° C. The reaction mixture was then concentrated and the aqueous suspension remaining was neutralized with 100 ml 1N HCl. The precipitate was filtered off, washed with water and dried overnight at 50° C. in a high vacuum. There were obtained 1.59 g of (RS)-(2-tert-butoxycarbonylmethoxy-3,5-dichloro-phenyl)-[4-(N-hydroxycarbamimidoyl)-phenylamino]-acetic acid; MS (ISP) m/z 484.3 (M+H)+, 506.2 (M+Na)+.

후처리

  1. concentrationThe reaction mixture was then concentrated
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customdried overnight at 50° C. in a high vacuum

출처 및 근거

ORD 기록
ord-c14f4340f9aa4757b8c21fec29ca5528
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07071212B2

반응 노트

불러오는 중…