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Sodium Azide → HCID 86609135, 화합물

HRID 902351
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HRID 902351 반응식
CC1C=CC(S(O[CH2:12][C@H:13]2[CH2:22][CH2:21][C:20]3[C:15](=[C:16]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[CH3:30])[C:17]([Cl:23])=[CH:18][CH:19]=3)[O:14]2)(=O)=O)=CC=1.[N-:31]=[N+:32]=[N-:33].[Na+]>CS(C)=O>[N:31]([CH2:12][C@H:13]1[CH2:22][CH2:21][C:20]2[C:15](=[C:16]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[CH3:30])[C:17]([Cl:23])=[CH:18][CH:19]=2)[O:14]1)=[N+:32]=[N-:33]
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참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 86609136HCID 86609136, 화합물

생성물 1

HCID 86609135HCID 86609135, 화합물수율 88.5%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
60 °C

실험 절차

To a solution of ((2R)-7-chloro-8-o-tolylchroman-2-yl)methyl 4-methylbenzenesulfonate (0.8 g, 1.8 mmol) in DMSO (50 mL) was added sodium azide (1.2 g, 18.4 mmol) and the resulting mixture was heated at 60° C. overnight. The mixture was extracted with ethyl acetate, washed with water and saturated sodium chloride, dried with anhydrous sodium sulfate and concentrated under reduced pressure. Purification by ISCO using a solvent gradient of 0 to 20% ethyl acetate in hexanes provided 0.5 g (88%) of (2R)-2-(azidomethyl)-7-chloro-8-o-tolylchroman as a colorless oil.

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. washwashed with water and saturated sodium chloride
  3. dry with materialdried with anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customPurification by ISCO

출처 및 근거

ORD 기록
ord-cef1c182e53a4ae283d52b6714334175
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07365095B2

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