Trifluoroacetic acid → HCID 21301010、化合物

HRID 49983

反応式

HRID 49983 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 21301010HCID 21301010、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-baad0f8c5728421b9d32f6e582adfc5c
出典データセット
uspto-grants-2004_03
特許番号
US06710064B2

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