Hydroxyamine hydrochloride → HCID 178452412、化合物

HRID 1514228ノート

反応式

HRID 1514228 の反応式
[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

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochloride2 回HCID 516892Sodium BicarbonateHCID 54757009Tert-butyl 9-cyano-2,3-dihydrobenzo[F][1,4]oxazepine-4(5H)-carboxylate

生成物 1

HCID 178452412HCID 178452412、化合物収率 69%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-c0d46a05387248558d159f24a420a158
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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