Phosphorus sulfide (P2S5) → Ethyl 2-[4-(5-fluorobenzothiazol-2-yl)methyl-3,4-dihydro-3-thioxo-2H-1,4-benzothiazin-2-yl]acetate

HRID 1655896ノート

反応式

HRID 1655896 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([CH2:10][N:11]3[C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=4[S:14][CH:13]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:12]3=O)=[N:7][C:6]=2[CH:28]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:30]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([CH2:10][N:11]3[C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=4[S:14][CH:13]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:12]3=[S:30])=[N:7][C:6]=2[CH:28]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 9909828Ethyl 2-[4-(5-fluorobenzothiazol-2-yl)methyl-3,4-dihydro-3-oxo-2H-1,4-benzothiazin-2-yl]acetate

生成物 1

HCID 10320610Ethyl 2-[4-(5-fluorobenzothiazol-2-yl)methyl-3,4-dihydro-3-thioxo-2H-1,4-benzothiazin-2-yl]acetate収率 71.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To 10 ml of toluene were added 720 mg of the compound of Example 1 and 770 mg of phosphorus pentasulfide. The mixture was heated to reflux for 4 hours. After the mixture has been cooled, the insoluble substance was filtered off and the solvent was distilled off. The residue was purified by silica gel chromatography to give 535 mg of the title compound. The structural formula and physical data of this compound are shown in Table 23.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4 hours
  3. temperatureAfter the mixture has been cooled
  4. filtrationthe insoluble substance was filtered off
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-bf57a48b69b34098ac87c74b1cc58048
出典データセット
uspto-grants-1993_10
特許番号
US05252571

反応ノート

読み込み中…