Hydrochloric Acid → HCID 178493668、化合物

HRID 37135

反応式

HRID 37135 の反応式
[H-].[Na+].[CH:3]([O:5][CH2:6][CH3:7])=O.[CH3:8][O:9]CC(OCC)=O.[NH2:16][C:17]1[C:21]([C:22]2[CH:27]=[CH:26][C:25]([S:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:24][CH:23]=2)=[CH:20][NH:19][N:18]=1.Cl>C(OCC)(=O)C.O.O1CCCC1>[OH:9][C:8]1[N:18]2[N:19]=[CH:20][C:21]([C:22]3[CH:23]=[CH:24][C:25]([S:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:26][CH:27]=3)=[C:17]2[N:16]=[CH:7][C:6]=1[O:5][CH3:3]

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 77544Ethyl 2-methoxyacetateHCID 178509258HCID 178509258、化合物

生成物 1

HCID 178493668HCID 178493668、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a tetrahydrofuran suspension of 480 mg of 60% sodium hydride, 2 ml of ethyl formate and 1.0 g of ethyl methoxyacetate were added under nitrogen atmosphere, and the mixture was stirred for 16 hours at room temperature. In succession, adding 1.0 g of 3-amino-4(4-phenylthiophenyl)pyrazole, the solution was stirred for 4 hours in reflux. After allowing to cool, water was added and the solution was neutralized with 10% hydrochloric acid. Removing water, ethyl acetate was added, and insoluble matter was filtered. The filtrate was washed in ethyl acetate and ether and dried, and the title compound was obtained (100 mg, 8%).

後処理

  1. additionwere added under nitrogen atmosphere
  2. stirringthe solution was stirred for 4 hours
  3. temperaturein reflux
  4. temperatureto cool
  5. filtrationinsoluble matter was filtered
  6. washThe filtrate was washed in ethyl acetate
  7. dry with materialether and dried

出典と根拠

ORDレコード
ord-907f2ec5246641ac9182ba93481bc4bb
出典データセット
uspto-grants-1995_05
特許番号
US05420128

関連ノート

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