Diethyl Ether → 1-(Aminooxy)-3,3-dimethylbutan-2-ol

HRID 494739노트

반응식

HRID 494739 반응식
[OH:1][CH:2]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:3][O:4][N:5]1C(=O)C2C(=CC=CC=2)C1=O.CNN.C(OCC)C>ClCCl>[NH2:5][O:4][CH2:3][CH:2]([OH:1])[C:16]([CH3:19])([CH3:18])[CH3:17]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 6061MethylhydrazineHCID 211115332-(2-Hydroxy-3,3-dimethylbutoxy)-isoindole-1,3-dione

생성물 1

HCID 211115321-(Aminooxy)-3,3-dimethylbutan-2-ol수율 86.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-(2-hydroxy-3,3-dimethylbutoxy)-isoindole-1,3-dione (1.47 g, 5.60 mmol) in dichloromethane (20 mL) cooled to 0° C. was added methylhydrazine (0.31 mL, 5.90 mmol). The white suspension was allowed to stir for 16 hours at room temperature. Diethyl ether (50 mL) was added and the solids were removed by filtration. The filtrate was concentrated, diluted with diethyl ether and the solids were removed by filtration. This procedure was repeated twice more and the final filtrate was concentrated to provide the desired product as a yellow liquid (0.643 g, 86%). 1H NMR (400 MHz, CDCl3) δ 4.87 (br s, 2H), 3.85 (q, 1H), 3.58 (q, 2H), 0.93 (s, 9H).

후처리

  1. customthe solids were removed by filtration
  2. concentrationThe filtrate was concentrated
  3. additiondiluted with diethyl ether
  4. customthe solids were removed by filtration
  5. concentrationthe final filtrate was concentrated

출처 및 근거

ORD 기록
ord-2ca3e4f120a2409a8e8d1a205e5f52a7
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538120B2

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