Trifluoroacetic acid → HCID 178480321、化合物

HRID 874077ノート

反応式

HRID 874077 の反応式
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][C@H:3]1[C:7]1[CH:8]=[C:9]([O:13][CH2:14][CH2:15][NH:16][C:17]([C@H:19]2[CH2:24][CH2:23][C@H:22]([NH:25]C(=O)OC(C)(C)C)[CH2:21][CH2:20]2)=[O:18])[CH:10]=[N:11][CH:12]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:25][C@H:22]1[CH2:21][CH2:20][C@H:19]([C:17]([NH:16][CH2:15][CH2:14][O:13][C:9]2[CH:10]=[N:11][CH:12]=[C:7]([C@@H:3]3[CH2:4][CH2:5][CH2:6][N:2]3[CH3:1])[CH:8]=2)=[O:18])[CH2:24][CH2:23]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 178480322HCID 178480322、化合物

生成物 1

HCID 178480321HCID 178480321、化合物収率 62.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of tert-butyl (trans-4-{[2-({5-[(2S)-1-methylpyrrolidin-2-yl]pyridin-3-yl}oxy)ethyl]carbamoyl}cyclohexyl)carbamate (preparation 35) (35 mg, 0.078 mmol) in DCM (3 mL) was treated with trifluoroacetic acid (1 mL). The resulting solution was stirred at ambient temperature overnight, after which time it was concentrated in vacuo. The residue was dissolved in MeOH and applied to an SCX-2 cartridge and eluted with MeOH followed by ammonia in MeOH (2M). The fractions containing product were concentrated in vacuo to give the title compound as an orange gum (17 mg, 62%).

後処理

  1. concentrationafter which time it was concentrated in vacuo
  2. dissolutionThe residue was dissolved in MeOH
  3. washeluted with MeOH
  4. additionThe fractions containing product
  5. concentrationwere concentrated in vacuo

出典と根拠

ORDレコード
ord-43326573e13a48cd88f4535dc1f37517
出典データセット
uspto-grants-2015_03
特許番号
US08980276B2

反応ノート

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