Potassium tert-butoxide → 7-Chloro-3,5-dihydrobenzo[e][1,4]oxazepin-2(1H)-one

HRID 528695노트

반응식

HRID 528695 반응식
Br[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[CH2:13][OH:14])=[O:4].CC(C)([O-])C.[K+]>CC(O)C>[Cl:12][C:9]1[CH:10]=[CH:11][C:6]2[NH:5][C:3](=[O:4])[CH2:2][O:14][CH2:13][C:7]=2[CH:8]=1

참가 물질

4

반응물 2

HCID 23665647Potassium tert-butoxideHCID 866797092-Bromo-N-(4-chloro-2-(hydroxymethyl)phenyl)acetamide

생성물 1

HCID 840481997-Chloro-3,5-dihydrobenzo[e][1,4]oxazepin-2(1H)-one수율 92%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a suspension of 2-bromo-N-(4-chloro-2-(hydroxymethyl)phenyl)acetamide (3.60 g, 12.9 mmol) in 2-propanol (129 ml) was added in small portions potassium tert-butoxide (3.77 g, 33.6 mmol) at 0-5° C. The reaction mixture was stirred for 90 minutes and then poured on ice/water (500 ml). The precipitate was collected by filtration and washed with water. Residual water was removed by evaporation of two 50 ml-portions of toluene to give the title compound (2.34 g, 92%) as light yellow solid. MS m/e: 196 ([M−H]−).

후처리

  1. additionpoured on ice/water (500 ml)
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customResidual water was removed by evaporation of two 50 ml-portions of toluene

출처 및 근거

ORD 기록
ord-bea87bc134fb43348181b4b40ee049e4
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346824B2

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