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Trifluoroacetic acid → [3-Chloro-4-(pyridin-2-ylmethoxy)-phenyl]-(5,6,7,8-tetrahydro-9-thia-1,3,7-triaza-fluoren-4-yl)amine

HRID 1887411
ノート
印刷プレビュー

反応式

HRID 1887411 の反応式
C(OC([N:8]1[CH2:20][C:19]2[S:18][C:17]3[N:16]=[CH:15][N:14]=[C:13]([NH:21][C:22]4[CH:27]=[CH:26][C:25]([O:28][CH2:29][C:30]5[CH:35]=[CH:34][CH:33]=[CH:32][N:31]=5)=[C:24]([Cl:36])[CH:23]=4)[C:12]=3[C:11]=2[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:36][C:24]1[CH:23]=[C:22]([NH:21][C:13]2[C:12]3[C:11]4[CH2:10][CH2:9][NH:8][CH2:20][C:19]=4[S:18][C:17]=3[N:16]=[CH:15][N:14]=2)[CH:27]=[CH:26][C:25]=1[O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][N:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 595869744-[3-Chloro-4-(pyridin-2-ylmethoxy)-phenylamino]-5,8-dihydro-6H-9-thia-1,3,7-triaza-fluorene-7-carboxylic acid tert-butyl ester

生成物 1

HCID 59586947[3-Chloro-4-(pyridin-2-ylmethoxy)-phenyl]-(5,6,7,8-tetrahydro-9-thia-1,3,7-triaza-fluoren-4-yl)amine収率 68.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a 4-[3-Chloro-4-(pyridin-2-ylmethoxy)-phenylamino]-5,8-dihydro-6H-9-thia-1,3,7-triaza-fluorene-7-carboxylic acid tert-butyl ester (3.6 g, 6.87 mmol) in DCM (45 mL) solution was added TFA (5.2 mL, 68.7 mmol, 10 equiv). The reaction mixture was stirred at rt for 8 h. The solution mixture was concentrated in vacuo. To the residue was added sat. NaHCO3 solution and stirred at rt for 1.5 h. The mixture was then filtered and washed with water. The damp solid was placed in a vacuum oven and dried for overnight to yield a yellow solid (2.0 g, 67%). 1H NMR (DMSO-d6) δ 9.41 (broad s, 2H), 8.71 (d, J=5.0 Hz, 1H), 8.40 (s, 1H), 8.11 (t, 1H), 7.75 (m, 2H), 7.57 (m, 1H), 7.53 (dd, J=2.7, 9.0 Hz, 1H), 7.25 (d, J=9.4 Hz, 1H), 5.35 (s, 2H), 4.48 (m, 2H), 3.49 (m, 2H), 3.41 (m, 2H); LCMS RT=2.11 min, [M+Na]+=446.1.

後処理

  1. concentrationThe solution mixture was concentrated in vacuo
  2. additionTo the residue was added sat. NaHCO3 solution
  3. stirringstirred at rt for 1.5 h
  4. filtrationThe mixture was then filtered
  5. washwashed with water
  6. customdried for overnight

出典と根拠

ORDレコード
ord-96ff19f1ddb5494f8d7810c03da41960
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501755B2

反応ノート

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