Methanesulfonyl chloride → tert-Butyl 2-((methylsulfonyl)oxy)-7-azaspiro[3.5]nonane-7-carboxylate

HRID 914818노트

반응식

HRID 914818 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:17][CH2:16][C:11]2([CH2:14][CH:13]([OH:15])[CH2:12]2)[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[CH2:9][CH2:10][C:11]2([CH2:12][CH:13]([O:15][S:19]([CH3:18])(=[O:21])=[O:20])[CH2:14]2)[CH2:16][CH2:17]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 9834677Tert-butyl 2-hydroxy-7-azaspiro[3.5]nonane-7-carboxylate

생성물 1

HCID 22248489tert-Butyl 2-((methylsulfonyl)oxy)-7-azaspiro[3.5]nonane-7-carboxylate수율 100%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

실험 절차

After dissolving 106 mg of 7-(tert-butoxycarbonyl)-2-hydroxy-7-azaspiro[3.5]nonane in 10 ml of tetrahydrofuran, 0.04 ml of methanesulfonyl chloride and 0.07 ml of triethylamine were 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 anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (148 mg, 100% yield).

후처리

  1. additionwere 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 anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-926ce589160e45e399540c48b26bdace
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265108B2

반응 노트

불러오는 중…