Hydrochloric Acid → HCID 178520244、化合物

HRID 1284646ノート

反応式

HRID 1284646 の反応式
[C:1]1([CH2:7][C:8]([NH:10][CH:11]2[C:37](=[O:38])[N:13]3[C:14]([C:21]([O:23][CH:24]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])=[C:15]([CH2:19]Cl)[CH2:16][S:17](=[O:18])[C@H:12]23)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH:39]1[C:43]([SH:44])=[N:42][N:41]=[N:40]1.CN(C)C=O.Cl>C(N(CC)CC)C>[C:1]1([CH2:7][C:8]([NH:10][CH:11]2[C:37](=[O:38])[N:13]3[C:14]([C:21]([O:23][CH:24]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])=[C:15]([CH2:19][S:44][C:43]4[NH:42][N:41]=[N:40][N:39]=4)[CH2:16][S:17](=[O:18])[C@H:12]23)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 13180407Benzhydryl 7-(2-phenylacetamido)-3-chloromethyl-3-cephem-4-carboxylate-1-oxideHCID 178527994HCID 178527994、化合物

生成物 1

HCID 178520244HCID 178520244、化合物収率 100.5%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

A mixture of benzhydryl 7-(2-phenylacetamido)-3-chloromethyl-3-cephem-4-carboxylate-1-oxide (70.0 g), 1H-tetrazole-5-thiol (15.6 g) and N,N-dimethylformamide (700 ml) was stirred to give a homogeneous solution and thereto was added triethylamine (32.1 g), keeping the temperature at 20° to 30° C. The resulting solution was stirred for 40 minutes at room temperature. After the reaction mixture was added to ice water (2.8 l), the mixture was adjusted to pH 2.0 with 10% hydrochloric acid and then filtered. The filter cake was washed with water and dried over phosphorus pentoxide under reduced pressure to give benzhydryl 7-(2-phenylacetamido)-3-(1H-tetrazole-5-yl)thiomethyl-3-cephem-4-carboxylate-1-oxide (78.8 g).

後処理

  1. customto give a homogeneous solution
  2. customat 20° to 30° C
  3. stirringThe resulting solution was stirred for 40 minutes at room temperature
  4. filtrationfiltered
  5. washThe filter cake was washed with water
  6. dry with materialdried over phosphorus pentoxide under reduced pressure

出典と根拠

ORDレコード
ord-e77479ee2a7c4e989d60ee7aa069143d
出典データセット
uspto-grants-1986_01
特許番号
US04563450

反応ノート

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