Di-tert-butyl dicarbonate → 1,1-dimethylethyl 9-[(phenylmethyl)oxy]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

HRID 1514222노트

반응식

HRID 1514222 반응식
[C:1]1([CH2:7][O:8][C:9]2[C:19]3[O:18][CH2:17][CH2:16][NH:15][CH2:14][C:13]=3[CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O:20](C(OC(C)(C)C)=O)[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=O>C(Cl)Cl>[C:1]1([CH2:7][O:8][C:9]2[C:19]3[O:18][CH2:17][CH2:16][N:15]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:20])[CH2:14][C:13]=3[CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 90495Di-tert-butyl dicarbonateHCID 594035049-[(Phenylmethyl)oxy]-2,3,4,5-tetrahydro-1,4-benzoxazepine

생성물 1

HCID 594034471,1-dimethylethyl 9-[(phenylmethyl)oxy]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

9-[(Phenylmethyl)oxy]-2,3,4,5-tetrahydro-1,4-benzoxazepine (Preparation 60) (7.01 g, 27.5 mmol) and BOC2O (7.01 ml, 30.2 mmol) were dissolved in DCM (100 ml) and left at room temperature for one hour then evaporated and biotage chromatographed in 5% EtOAc in hexane to remove excess BOC2O and changing to 15% EtOAc in iso-hexane to elute the title compound (8.25 g) as a white solid. MS (ES): C21H25NO4 requires 355; found 256 [M+H−100]+.

후처리

  1. customthen evaporated
  2. custombiotage chromatographed in 5% EtOAc in hexane
  3. customto remove excess BOC2O
  4. washto elute the title compound (8.25 g) as a white solid

출처 및 근거

ORD 기록
ord-5f2dff7c2db74f0dab078b66c526f37e
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222245B2

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