Methanesulfonyl chloride → HCID 22248366, 화합물

HRID 914817노트

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HRID 914817 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([C:16]#[N:17])([CH2:14][OH:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:18][S:19](Cl)(=[O:21])=[O:20]>O1CCCC1.C(N(CC)CC)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([C:16]#[N:17])([CH2:14][O:15][S:19]([CH3:18])(=[O:21])=[O:20])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 222486071-Boc-4-cyano-4-(hydroxymethyl)piperidine

생성물 1

HCID 22248366HCID 22248366, 화합물수율 100%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

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온도
0 °C

실험 절차

After dissolving 537 mg of 1-(tert-butoxycarbonyl)-4-cyano-4-(hydroxymethyl)piperidine in 100 ml of tetrahydrofuran, 0.4 ml of triethylamine was added and the solution was cooled to 0° C. 0.2 ml of methanesulfonyl chloride was added and the mixture was stirred overnight at room temperature. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. After adding water to the residue, extraction was performed with ethyl acetate. The organic layer was washed with water and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (799 mg, 100% yield).

후처리

  1. additionwas added
  2. filtrationThe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionAfter adding water
  5. extractionto the residue, extraction
  6. washThe organic layer was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b65abf4371f046048e2550caf6a67809
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265108B2

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