Hydrochloric Acid → HCID 7174615、化合物

HRID 1054318ノート

反応式

HRID 1054318 の反応式
[CH3:1][C:2]1[C:10]2[C:9]([C:11]([O:13]C)=[O:12])=[CH:8][C:7]([CH3:15])=[N:6][C:5]=2[N:4]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:3]=1.Cl>>[CH3:1][C:2]1[C:10]2[C:9]([C:11]([OH:13])=[O:12])=[CH:8][C:7]([CH3:15])=[N:6][C:5]=2[N:4]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:3]=1

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 17025734methyl 3,6-dimethyl-1-phenylpyrazolo[3,4-b]pyridine-4-carboxylate

生成物 1

HCID 7174615HCID 7174615、化合物収率 81%

実験手順

Synthesized using the procedure for 1 except ester 46 was used as the starting material. After the work up and acidifying the aqueous layer with 1N HCl, solid precipitated which was filtered off and dried on high vacuum to provide the title compound (165 mg, 81%) as a light yellow solid. 100% pure by HPLC. 1H NMR (400 MHz, DMSO-d6) δ 13.90 (s, 1H), 8.19 (d, J=7.7 Hz, 2H), 7.56-7.48 (m, 3H), 7.29 (t, J=7.3 Hz, 1H), 2.65 (s, 3H), 2.63 (s, 3H). 13C NMR (100 MHz, DMSO-d6) δ 167.04, 159.52, 151.67, 142.43, 139.35, 135.32, 129.49, 126.12, 121.13, 118.29, 111.04, 24.92, 16.12. ESI MS: m/z 268.1 (M+H)+.

後処理

  1. customSynthesized
  2. customprecipitated which
  3. filtrationwas filtered off
  4. customdried on high vacuum

出典と根拠

ORDレコード
ord-fbaebd89cebc4935a66b8e06944e2e76
出典データセット
uspto-grants-2016_07
特許番号
US09394303B2

反応ノート

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