Trifluoroacetic acid → HCID 67487214、化合物

HRID 1809622ノート

反応式

HRID 1809622 の反応式
[CH3:1][C:2]1[C:7]([O:8][C:9]2[C:10]([NH:22][C:23]3[S:27][N:26]=[C:25]([CH:28]4[CH2:34][CH:33]5[N:35](C(OC(C)(C)C)=O)[CH:30]([CH2:31][CH2:32]5)[CH2:29]4)[N:24]=3)=[N:11][CH:12]=[C:13]([S:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=3)[CH:14]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH:30]12[NH:35][CH:33]([CH2:32][CH2:31]1)[CH2:34][CH:28]([C:25]1[N:24]=[C:23]([NH:22][C:10]3[C:9]([O:8][C:7]4[C:2]([CH3:1])=[N:3][CH:4]=[CH:5][CH:6]=4)=[CH:14][C:13]([S:15][C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=4)=[CH:12][N:11]=3)[S:27][N:26]=1)[CH2:29]2

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 68710136HCID 68710136、化合物

生成物 1

HCID 67487214HCID 67487214、化合物収率 95.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 3-(5-(3-(2-methylpyridin-3-yloxy)-5-(pyridin-2-ylthio)pyridin-2-ylamino)-1,2,4-thiadiazol-3-yl)-8-azabicyclo[3.2.1]octane-8-carboxylate (550 mg, 0.911 mmol) was dissolved in CH2Cl2 (2 mL) and TFA (1 mL) was added and the reaction was stirred for 45 minutes. The reaction was partitioned between saturated aqueous NaHCO3 and CH2Cl2, dried over sodium sulfate, filtered and concentrated to afford 3-(8-azabicyclo[3.2.1]octan-3-yl)-N-(3-(2-methylpyridin-3-yloxy)-5-(pyridin-2-ylthio)pyridin-2-yl)-1,2,4-thiadiazol-5-amine (438 mg, 0.870 mmol, 95.5% yield).

後処理

  1. customThe reaction was partitioned between saturated aqueous NaHCO3 and CH2Cl2
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-7e0333a17ea5437c987c6283dd4caacb
出典データセット
uspto-grants-2013_01
特許番号
US08362037B2

反応ノート

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