Zopiclone → (S)-Zopiclone Besylate

HRID 454829

반응식

HRID 454829 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C@@H:11]2[N:20]([C:21]3[CH:22]=[CH:23][C:24]([Cl:27])=[CH:25][N:26]=3)[C:18](=[O:19])[C:13]3[N:14]=[CH:15][CH:16]=[N:17][C:12]2=3)=[O:9])[CH2:4][CH2:3]1.[C:28]1([S:34]([OH:37])(=[O:36])=[O:35])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.CN1CCN(C(OC2N(C3C=CC(Cl)=CN=3)C(=O)C3N=CC=NC2=3)=O)CC1>O1CCCC1>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C@@H:11]2[N:20]([C:21]3[CH:22]=[CH:23][C:24]([Cl:27])=[CH:25][N:26]=3)[C:18](=[O:19])[C:13]3[N:14]=[CH:15][CH:16]=[N:17][C:12]2=3)=[O:9])[CH2:4][CH2:3]1.[S:34]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)([O-:37])(=[O:36])=[O:35]

참가 물질

5

반응물 3

HCID 5735ZopicloneHCID 7371Benzenesulfonic AcidHCID 969472Eszopiclone

생성물 1

HCID 131729769(S)-Zopiclone Besylate수율 92.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
35 °C

실험 절차

A 2000 mL reactor was charged with 10.0 g (S)-zopiclone and 400 mL tetrahydrofuran (THF). The contents were heated to 35° C. Into a 1000 mL reactor was charged 4.4 g benzenesulfonic acid and 400 mL THF, and stirred until a solution was formed. The acid solution was transferred slowly to the zopiclone solution. The reaction was cooled to 15° C. and stirred for 18 hr at 20-25° C. The reactor slurry was filtered and washed with THF in an appropriate filter. The wet cake was dried under vacuum at 60-65° C. and packaged in an appropriate container. Isolated yield=92.7%.

후처리

  1. customwas formed
  2. temperatureThe reaction was cooled to 15° C.
  3. stirringstirred for 18 hr at 20-25° C
  4. filtrationThe reactor slurry was filtered
  5. washwashed with THF in an appropriate filter
  6. customThe wet cake was dried under vacuum at 60-65° C.
  7. customIsolated yield=92.7%

출처 및 근거

ORD 기록
ord-bfe88e8f1e17489882f240f8f4f9daaf
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497267B2

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