Methanesulfonamide → N-(cyclopropylmethylene)methanesulfonamide

HRID 2407442

반응식

HRID 2407442 반응식
[CH:1]1([CH:4]=O)[CH2:3][CH2:2]1.[CH3:6][S:7]([NH2:10])(=[O:9])=[O:8]>C1(C)C=CC=CC=1.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[CH:1]1([CH:4]=[N:10][S:7]([CH3:6])(=[O:9])=[O:8])[CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 72879MethanesulfonamideHCID 123114Cyclopropanecarboxaldehyde

생성물 1

HCID 66788560N-(cyclopropylmethylene)methanesulfonamide

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

To a solution of cyclopropanecarbaldehyde (0.374 mL, 5 mmol) and methanesulfonamide (0.523 g, 5.5 mmol) in toluene (15 mL) was added titanium(IV) isopropoxide (2.93 mL, 10 mmol), and the mixture was heated to 100° C. for 1 day. The mixture was cooled to room temperature and concentrated in vacuo. The residue was placed under high vacuum for 30 min to give a biphasic mixture. The top layer was discarded. The residue was used in next step without further purification.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated in vacuo
  3. customto give a biphasic mixture
  4. customThe residue was used in next step without further purification

출처 및 근거

ORD 기록
ord-84149e9e913b4034acc523b218491be1
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809545B2

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