Trichloroacetyl isocyanate → HCID 14556140、化合物

HRID 745967ノート

反応式

HRID 745967 の反応式
[Cl:1][C:2]([Cl:9])([Cl:8])[C:3]([N:5]=[C:6]=[O:7])=[O:4].[OH:10][CH2:11][C:12]1[CH2:13][S:14][C@@H:15]2[C@H:22]([NH:23][C:24](=[O:31])[CH2:25][C:26]3[S:27][CH:28]=[CH:29][CH:30]=3)[C:21](=[O:32])[N:16]2[C:17]=1[C:18]([OH:20])=[O:19]>C(OCC)(=O)C>[S:27]1[CH:28]=[CH:29][CH:30]=[C:26]1[CH2:25][C:24]([NH:23][C@@H:22]1[C:21](=[O:32])[N:16]2[C:17]([C:18]([OH:20])=[O:19])=[C:12]([CH2:11][O:10][C:6](=[O:7])[NH:5][C:3](=[O:4])[C:2]([Cl:9])([Cl:8])[Cl:1])[CH2:13][S:14][C@H:15]12)=[O:31]

参加物

4

反応物 2

HCID 76400Trichloroacetyl isocyanateHCID 93015Deacetylcephalothin

生成物 1

HCID 14556140HCID 14556140、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Trichloroacetylisocyanate (4.3 ml) was added rapidly to a stirred suspension of (6R,7R)-3-hydroxymethyl-7-(2-thienylacetamido)ceph-3-em-4-carboxylic acid (10.62 g) at 6° in ethyl acetate (70 ml). The reaction mixture was stirred at 5° for 40 min. Petroleum ether was added dropwise during 15 min. The mixture was stirred for 30 min, filtered and the solid was washed with petroleum ether and dried to give the title compound as a solid (16.48 g), [α]D22 +73° (c 1.2 in Me2SO).

後処理

  1. stirringThe mixture was stirred for 30 min
  2. filtrationfiltered
  3. washthe solid was washed with petroleum ether
  4. customdried

出典と根拠

ORDレコード
ord-b961cb4450504efd8ca8a78f04f61b05
出典データセット
uspto-grants-1986_07
特許番号
US04602012

反応ノート

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