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Morpholine → HCID 13013938, 화합물

HRID 444152
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HRID 444152 반응식
Cl[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:12][C:7]=2[S:6](=[O:18])(=[O:17])[C:5]2[CH:19]=[CH:20][CH:21]=[CH:22][C:4]=2[N:3]=1.[NH:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>C(#N)C>[O:26]1[CH2:27][CH2:28][N:23]([C:2]2[C:8]3[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:12][C:7]=3[S:6](=[O:18])(=[O:17])[C:5]3[CH:19]=[CH:20][CH:21]=[CH:22][C:4]=3[N:3]=2)[CH2:24][CH2:25]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 13013934HCID 13013934, 화합물

생성물 1

HCID 13013938HCID 13013938, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Reflux a mixture of 5.025 mg (15 mmole) of the 11-chloro ester of Example 14. 3.119 gm of morpholine and 75 ml of acetonitrile for 2 hours. Distill off the acetonitrile under a vacuum and dissolve the residue in 45 ml of methanol at room temperature. Filter, cool and separate the precipitate by filtration. Chromatograph over silica gel eluting with 1:4 ethylacetate in toluene. Recrystallize from ethanol to obtain the title product (m.p. 164°-166° C.).

후처리

temperature
Reflux
  • distillationDistill off the acetonitrile under a vacuum
  • dissolutiondissolve the residue in 45 ml of methanol at room temperature
  • filtrationFilter
  • temperaturecool
  • customseparate the precipitate
  • filtrationby filtration
  • customRecrystallize from ethanol
  • 출처 및 근거

    ORD 기록
    ord-a9c2c117ade44022800943b61dd76726
    출처 데이터셋
    uspto-grants-1981_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04263207

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