Lithium Carbonate → HCID 178451342、化合物

HRID 1016799ノート

反応式

HRID 1016799 の反応式
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]

参加物

5

反応物 2

HCID 11125Lithium CarbonateHCID 178501559HCID 178501559、化合物

生成物 1

HCID 178451342HCID 178451342、化合物収率 83.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
57.5 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-7de0abd745134394a4f37c6b09ed2feb
出典データセット
uspto-grants-2002_11
特許番号
US06476264B2

反応ノート

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