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

HRID 1655896노트

반응식

HRID 1655896 반응식
[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

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bf57a48b69b34098ac87c74b1cc58048
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05252571

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