Ammonia → HCID 23464473、化合物
反応式
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([C:13](OC)=O)=[CH:12][C:7]=2[S:6][C:5]2[CH:17]=[CH:18][CH:19]=[CH:20][C:4]=2[NH:3]1.[NH3:21]>CO>[C:13]([C:11]1[CH:10]=[CH:9][C:8]2[C:2](=[O:1])[NH:3][C:4]3[CH:20]=[CH:19][CH:18]=[CH:17][C:5]=3[S:6][C:7]=2[CH:12]=1)#[N:21]参加物
4
実験手順
Stir 5 gm. of methyl 10,11-dihydro-11-oxodibenzo[b,f][1,4]thiazepin-3-carboxylate in 500 ml. of methanol saturated with ammonia gas for 24 hours at room temperature. Evaporate the reaction mixture to dryness. Reflux the residue in 200 ml. of methylene chloride containing 10 gm. of phosphorous oxychloride for eight hours. Cool the reaction mixture to room temperature and shake several times with water. Separate the organic layer, dry over magnesium sulfate and evaporate to dryness to obtain the title product.
後処理
- customEvaporate the reaction mixture to dryness
- temperatureReflux the residue in 200 ml
- customSeparate the organic layer
- dry with materialdry over magnesium sulfate
- customevaporate to dryness
出典と根拠
- ORDレコード
- ord-f5a745771f5540d38ed29dcacb826d1a
- 出典データセット
- uspto-grants-1981_04
- 特許番号
- US04263207
反応ノート
読み込み中…