Trifluoroacetic acid → 1-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane

HRID 1434567ノート

反応式

HRID 1434567 の反応式
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][CH2:25][N:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[N:26]1([CH2:25][CH2:24][CH2:23][O:22][C:19]2[CH:20]=[CH:21][C:16]([CH2:15][N:11]3[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]3)=[CH:17][CH:18]=2)[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 102964254-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane-1-carboxylic acid tert-butyl ester

生成物 1

HCID 596405921-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane収率 89.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-[4-(3-Piperidin-1-yl-propoxy)-benzyl]-[1,4]diazepane-1-carboxylic acid tert-butyl ester (D3) (2.27 g, 5.27 mmol) was dissolved in dichloromethane (10 ml), treated with trifluoroacetic acid (5 ml) and stirred at room temperature under argon for 2 hours. The solvent was removed in vacuo and the residue dissolved in methanol and passed down an SCX column (10 g) eluting with methanol followed by 0.88 ammonia/methanol (1:9). The basic fractions were combined and concentrated in vacuo to afford the title compound (1.57 g).

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in methanol
  3. washeluting with methanol
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-143a97be32394813984dc4f3a46bc604
出典データセット
uspto-grants-2009_11
特許番号
US07615550B2

反応ノート

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