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

HRID 1514222ノート

反応式

HRID 1514222 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-5f2dff7c2db74f0dab078b66c526f37e
出典データセット
uspto-grants-2012_07
特許番号
US08222245B2

反応ノート

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