Trifluoroacetic acid → 6-Amino-1-(2,3-difluorobenzyl)-4-(2,2,2-trifluoroethyl)-1,4-diazepan-5-one

HRID 271967

反応式

HRID 271967 の反応式
FC(F)(F)C(O)=O.[F:8][C:9]1[C:36]([F:37])=[CH:35][CH:34]=[CH:33][C:10]=1[CH2:11][N:12]1[CH2:18][CH:17]([NH:19]C(=O)OC(C)(C)C)[C:16](=[O:27])[N:15]([CH2:28][C:29]([F:32])([F:31])[F:30])[CH2:14][CH2:13]1>ClCCl>[NH2:19][CH:17]1[CH2:18][N:12]([CH2:11][C:10]2[CH:33]=[CH:34][CH:35]=[C:36]([F:37])[C:9]=2[F:8])[CH2:13][CH2:14][N:15]([CH2:28][C:29]([F:31])([F:32])[F:30])[C:16]1=[O:27]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 68433007tert-Butyl 1-(2,3-difluorobenzyl)-5-oxo-4-(2,2,2-trifluoroethyl)-1,4-diazepan-6-ylcarbamate

生成物 1

HCID 222932496-Amino-1-(2,3-difluorobenzyl)-4-(2,2,2-trifluoroethyl)-1,4-diazepan-5-one収率 94%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (2.5 mL) was added to a solution of tert-butyl 1-(2,3-difluorobenzyl)-5-oxo-4-(2,2,2-trifluoroethyl)-1,4-diazepan-6-ylcarbamate (62 mg, 0.142 mmol) in dichloromethane (5 mL). After I h, the solution was concentrated. Saturated aqueous sodium bicarbonate solution was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with saturated brine, dried over magnesium sulfate, filtered and concentrated to give the title compound (45 mg). MS 338 (M+1).

後処理

  1. concentrationAfter I h, the solution was concentrated
  2. additionSaturated aqueous sodium bicarbonate solution was added
  3. extractionthe mixture was extracted with dichloromethane (3×)
  4. washThe combined organic extracts were washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-a45656a9054b4f0798b9bd1c3a2149b2
出典データセット
uspto-grants-2008_11
特許番号
US07452903B2

関連ノート

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