Butylamine → HCID 178448983, 화합물

HRID 254534노트

반응식

HRID 254534 반응식
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[CH:4]=O.[CH2:11]([NH2:15])[CH2:12][CH2:13][CH3:14]>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH2:11](/[N:15]=[CH:4]/[C:3]1[C:2]([F:1])=[CH:9][CH:8]=[CH:7][C:6]=1[F:10])[CH2:12][CH2:13][CH3:14]

참가 물질

6

반응물 2

HCID 8007ButylamineHCID 1362842,6-Difluorobenzaldehyde

생성물 1

HCID 178448983HCID 178448983, 화합물수율 86.1%

시약·촉매·용매 3

HCID 6101p-Toluenesulfonic acid촉매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 25.4 g (179 mmol) 2,6-difluorobenzaldehyde, 19.5 ml (197 mmol) N-butylamine and 0.68 g (3.57 mmol) p-toluenesulfonic acid in 120 ml toluene was heated in a Dean-Stark apparatus at reflux for 3 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and washed sequentially with water (twice) and with saturated brine. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo to afford the title compound 30.4 g (86%) as a brown oil which was used in the next step without further purification. MS (ISP): 198.3 ([M+H]+, 100%).

후처리

  1. temperaturewas heated in a Dean-Stark apparatus
  2. temperatureat reflux for 3 hours
  3. washwashed sequentially with water (twice) and with saturated brine
  4. dry with materialThe organic phase was dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-80a29760f07746cd8884e0fca3e57ba8
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875645B2

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