Hydroxyamine hydrochloride → HCID 178452412, 화합물

HRID 1514228노트

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HRID 1514228 반응식
[C:1]([C:3]1[C:13]2[O:12][CH2:11][CH2:10][N:9]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2].Cl.[NH2:22][OH:23].C(=O)(O)[O-].[Na+]>C(O)C>[OH:23][NH:22][C:1](=[NH:2])[C:3]1[C:13]2[O:12][CH2:11][CH2:10][N:9]([C:14]([O:16][C:17]([CH3:19])([CH3:18])[CH3:20])=[O:15])[CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochloride2회HCID 516892Sodium BicarbonateHCID 54757009Tert-butyl 9-cyano-2,3-dihydrobenzo[F][1,4]oxazepine-4(5H)-carboxylate

생성물 1

HCID 178452412HCID 178452412, 화합물수율 69%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

A suspension of 1,1-dimethylethyl 9-cyano-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (Preparation 64) (5.1 g, 18.59 mmol), hydroxylamine hydrochloride (2.58 g, 37.2 mmol) and sodium bicarbonate (7.81 g, 93 mmol) in ethanol (50 ml) was heated at 60° C. overnight. A further portion of hydroxylamine hydrochloride (1 g) was added and the reaction was heated at 60° C. overnight. The solid was filtered from the reaction mixture and the filtrate evaporated. The residue from the evaporation was dissolved in EtOAc, washed with water, dried over magnesium sulphate and evaporated. Trituration with ether to gave the title compound (3.94 g) as a white solid. MS (ES): C15H21N3O4 requires 307; found 308 [M+H]+.

후처리

  1. temperaturethe reaction was heated at 60° C. overnight
  2. filtrationThe solid was filtered from the reaction mixture
  3. customthe filtrate evaporated
  4. customThe residue from the evaporation
  5. dissolutionwas dissolved in EtOAc
  6. washwashed with water
  7. dry with materialdried over magnesium sulphate
  8. customevaporated

출처 및 근거

ORD 기록
ord-c0d46a05387248558d159f24a420a158
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222245B2

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