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HCID 59490356、化合物 → HCID 59490577、化合物

HRID 2383489
ノート
印刷プレビュー

反応式

HRID 2383489 の反応式
COC1C=CC(C[N:8]2[C:12]3[N:13]=[CH:14][C:15]4[CH2:16][CH:17]([C:21]([NH:23][C:24]5[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=5)=[O:22])[CH2:18][CH2:19][C:20]=4[C:11]=3[CH:10]=[N:9]2)=CC=1>FC(F)(F)C(O)=O>[C:24]1([NH:23][C:21]([CH:17]2[CH2:16][C:15]3[CH:14]=[N:13][C:12]4[NH:8][N:9]=[CH:10][C:11]=4[C:20]=3[CH2:19][CH2:18]2)=[O:22])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 59490356HCID 59490356、化合物

生成物 1

HCID 59490577HCID 59490577、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 3-(4-Methoxybenzyl)-N-phenyl-6,7,8,9-tetrahydro-3H-pyrazolo[3,4-c]isoquinoline-7-carboxamide in trifluoroacetic acid (5 mL) was heated at 65° C. for 8 hours. The mixture was evaporated to dryness and partitioned between ethyl acetate (100 mL) and saturated sodium hydrogen carbonate (100 mL). The organic layer was dried with anhydrous magnesium sulfate and evaporated under reduced pressure the residue obtained was triturated with dichloromethane (2 mL) to give N-phenyl-6,7,8,9-tetrahydro-3H-pyrazolo[3,4-c]isoquinoline-7-carboxamide as a white powder (10 mg). M.p.=>300° C. 1H NMR (DMSO-d6) 400 MHz δ 13.30 (s, 1H), 10.05 (s, 1H), 8.0 (s, 1H), 7.95 (s, 1H), 7.63 (d, J=7.6 Hz, 2H), 7.31 (t, J=7.6 Hz, 2H), 7.04 (t, J=7.6 Hz, 1H), 3.09-3.00 (m, 4H), 2.96-2.81 (m, 1H), 2.19-2.17 (m, 1H), 2.03-1.93 (m, 1H). LCMS [M+H]: 293.

後処理

  1. customThe mixture was evaporated to dryness
  2. custompartitioned between ethyl acetate (100 mL) and saturated sodium hydrogen carbonate (100 mL)
  3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  4. customevaporated under reduced pressure the residue
  5. customobtained
  6. customwas triturated with dichloromethane (2 mL)

出典と根拠

ORDレコード
ord-a9874afbebf44ce7ab936fa9324efcf0
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263610B2

反応ノート

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