Dimethylamine → HCID 15042213, 화합물

HRID 2371742노트

반응식

HRID 2371742 반응식
[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[O:4][CH:5]1[CH2:8][N:7]([C:9](Cl)=[O:10])[CH2:6]1.[CH3:17][NH:18][CH3:19]>O1CCCC1.O>[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[O:4][CH:5]1[CH2:8][N:7]([C:9]([N:18]([CH3:19])[CH3:17])=[O:10])[CH2:6]1

참가 물질

5

반응물 2

HCID 674DimethylamineHCID 199062193-(2,4-Dichlorophenoxy)-1-azetidinecarbonyl chloride

생성물 1

HCID 15042213HCID 15042213, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of 4.8 g (0.017 mole) of 3-(2,4-dichlorophenoxy)-1-azetidinecarbonyl chloride in 20 mL of tetrahydrofuran was treated with 5.8 mL (0.05 mole) of 40% aqueous dimethylamine. After stirring for 5 h, the reaction mixture was diluted with 200 mL of water and the oil which separated was extracted into methylene chloride (3×30 mL). The combined extracts were dried (Whatman PS paper) and concentrated in vacuo, (5 g). The crude oil solidified on standing and was recrystallized from ligroin yielding 3.4 g (69.2%) of silver plate-like crystals, mp 62°-63° C.

후처리

  1. customthe oil which separated
  2. extractionwas extracted into methylene chloride (3×30 mL)
  3. customThe combined extracts were dried (Whatman PS paper)
  4. concentrationconcentrated in vacuo, (5 g)
  5. customwas recrystallized from ligroin yielding 3.4 g (69.2%) of silver plate-like crystals, mp 62°-63° C.

출처 및 근거

ORD 기록
ord-005ca715f5074b3fa087a638a1cf9521
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05095014

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