Sodium Azide → HCID 86639452, 화합물

HRID 451831노트

반응식

HRID 451831 반응식
[N-:1]=[N+:2]=[N-:3].[Na+].CC1C=CC(S(O[CH2:16][C@@H:17]([NH:26][C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:18][C@H:19]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21][CH2:20]2)(=O)=O)=CC=1>CN(C=O)C.CCOC(C)=O>[N:1]([CH2:16][C@@H:17]([NH:26][C:27](=[O:28])[O:29][C:30]([CH3:33])([CH3:32])[CH3:31])[CH2:18][C@@H:19]1[CH2:25][CH2:24][CH2:23][CH2:22][O:21][CH2:20]1)=[N+:2]=[N-:3]

참가 물질

5

반응물 2

HCID 33557Sodium AzideHCID 59201342HCID 59201342, 화합물

생성물 1

HCID 86639452HCID 86639452, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

The solution of NaN3 (47 mg, 0.72 mmol) and (S)-2-(tert-butoxycarbonylamino)-3-((R)-oxepan-3-yl)propyl 4-methylbenzenesulfonate (103 mmol, 0.24 mmol) in anhydrous DMF was heated to 80° C. for 2 h. After cooling to rt, the reaction was diluted with EtOAc and washed with H2O, brine, dried over Na2SO4, filtered, and concentrated. The residue was purified by chromatography on silica gel to give tert-butyl (S)-1-azido-3-((S)-oxepan-3-yl)propan-2-ylcarbamate. MS ESI +ve m/z 321 (M+Na).

후처리

  1. washwashed with H2O, brine
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-e1c9c572d6ab47da9cf07f678ceae67f
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08487108B2

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