Trifluoroacetic acid → HCID 21301010, 화합물

HRID 49983

반응식

HRID 49983 반응식
C(O)(C(F)(F)F)=O.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][N:17]([CH2:23]OC)[CH2:18][Si](C)(C)C)=[CH:11][CH:10]=1.[Cl:26][C:27]1[CH:28]=[C:29]([N:34]2[C:38](=[O:39])[CH2:37][CH2:36][C:35]2=[O:40])[CH:30]=[C:31]([Cl:33])[CH:32]=1>C(Cl)Cl>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][CH2:16][N:17]2[CH2:18][CH:37]3[C:38](=[O:39])[N:34]([C:29]4[CH:28]=[C:27]([Cl:26])[CH:32]=[C:31]([Cl:33])[CH:30]=4)[C:35](=[O:40])[CH:36]3[CH2:23]2)=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 90363DimethachlonHCID 213010074-Chloro-N-(methoxymethyl)-N-[(trimethylsilyl)methyl]benzeneethanamine

생성물 1

HCID 21301010HCID 21301010, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To prepare the compound of formula (Im), wherein R11 is chloro and m is 2, TFA (32 μl, 0.41 mmol) was added to an ice-cooled mixture of 4-chloro-N-(methoxymethyl)-N-[(trimethylsilyl)methyl]benzeneethanamine (1.5 g, 5.25 mmol) (Preparation 14) and N-(3,5-dichlorophenyl)succinimide (1 g, 4.13 mmol, prepared according to Fujinami et al., Agr. Biol. Chem. [1972], p. 318, incorporated herein by reference) in methylene chloride (10 mL). The reaction mixture was allowed to warm to RT over 3 h. The solution was washed with ammonium hydroxide. The organic layer was dried over MgSO4 and concentrated in vacuo to afford after chromatography over silica gel (CH2Cl2) the above-referenced compound as a white solid (1.56 g). Mp=115° C. 1H NMR (CDCl3): 7.40 (1H, br s), 7.15-7.35 (4H, m), 7.07 (2H, d, J=8.3 Hz), 3.4-3.5 (2H, m), 3.3-3.4 (2H, m), 2.55-2.8 (4H, m), 2.35-2.5 (2H, m).

후처리

  1. customTo prepare the compound of formula (Im), wherein R11
  2. temperaturecooled
  3. customprepared
  4. washThe solution was washed with ammonium hydroxide
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-baad0f8c5728421b9d32f6e582adfc5c
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710064B2

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