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p-Toluenesulfonic acid monohydrate → HCID 86599621, 화합물

HRID 505442
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HRID 505442 반응식
C(OC([N:8]1[CH2:12][C@H:11]([OH:13])[CH2:10][C@H:9]1[C:14]#[N:15])=O)(C)(C)C.O.[CH3:17][C:18]1[CH:23]=[CH:22][C:21]([S:24]([OH:27])(=[O:26])=[O:25])=[CH:20][CH:19]=1>C(#N)C>[OH:13][C@H:11]1[CH2:12][NH:8][C@H:9]([C:14]#[N:15])[CH2:10]1.[CH3:17][C:18]1[CH:19]=[CH:20][C:21]([S:24]([O-:27])(=[O:26])=[O:25])=[CH:22][CH:23]=1
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참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 24903573(2S,4R)-1-Boc-2-cyano-4-hydroxypyrrolidine

생성물 1

HCID 86599621HCID 86599621, 화합물수율 74.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

6.40 g (30 mmol) of (2S,4R)-1-(tert-butoxycarbonyl)-4-hydroxy-pyrrolidine-2-carbonitrile was dissolved in 100 ml of acetonitrile and 8.56 g (45 mmol) of 4-methylbenzenesulphonic acid monohydrate was added to the solution. The mixture was stirred at room temperature for 24 hours and was evaporated under reduced pressure. 500 ml of diethyl ether was added to the resulting brown oil. It was stirred 10 minutes and kept in the refrigerator for a night. The resulting white crystalline material was filtered off and washed with diethyl ether. 6.31 g (73%) of the above product are obtained. M.p.: 110-113° C.

후처리

  1. customwas evaporated under reduced pressure
  2. addition500 ml of diethyl ether was added to the resulting brown oil
  3. stirringIt was stirred 10 minutes
  4. waitkept in the refrigerator for a night
  5. filtrationThe resulting white crystalline material was filtered off
  6. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-2cda63b4719f4cb3886697187a10367a
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07781455B2

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