Ammonia → HCID 86689764、化合物

HRID 1396414ノート

反応式

HRID 1396414 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([C:8](OCC)=[O:9])=[C:4]([NH:13][C:14]2[N:19]=[C:18]3[CH2:20][CH2:21][CH2:22][C:17]3=[CH:16][CH:15]=2)[CH:3]=1.CO.[NH3:25]>>[Cl:1][C:2]1[N:7]=[N:6][C:5]([C:8]([NH2:25])=[O:9])=[C:4]([NH:13][C:14]2[N:19]=[C:18]3[CH2:20][CH2:21][CH2:22][C:17]3=[CH:16][CH:15]=2)[CH:3]=1

参加物

4

反応物 3

HCID 222AmmoniaHCID 887MethanolHCID 86689763ethyl 6-chloro-4-(6,7-dihydro-5H-cyclopenta[b]pyridin-2-ylamino)pyridazine-3-carboxylate

生成物 1

HCID 86689764HCID 86689764、化合物収率 75%

実験手順

Ethyl 6-chloro-4-(6,7-dihydro-5H-cyclopenta[b]pyridin-2-ylamino)pyridazine-3-carboxylate (554 mg, 1.74 mmol) was suspended in ammonia 7M in methanol (11.8 g, 15.0 mL, 105 mmol). The flask containing the mixture was sealed and stirred at room temperature for 18 h. The precipitated off-white solid was separated by filtration and dried under high vacuum to give 6-chloro-4-(6,7-dihydro-5H-cyclopenta[b]pyridin-2-ylamino)pyridazine-3-carboxamide (375 mg, 75%) as an off-white solid. 1H NMR (DMSO-d6) δ: 11.92 (s, 1H), 8.95 (s, 1H), 8.83 (s, 1H), 8.18 (s, 1H), 7.63 (d, J=7.9 Hz, 1H), 6.84 (d, J=7.9 Hz, 1H), 2.78-3.00 (m, 4H), 2.07 (quin, J=7.6 Hz, 2H); LC-MS 290.0 [M+H]+.

後処理

  1. additionThe flask containing the mixture
  2. customwas sealed
  3. customThe precipitated off-white solid was separated by filtration
  4. customdried under high vacuum

出典と根拠

ORDレコード
ord-6e6d937eded14545be4ce2503a8766bb
出典データセット
uspto-grants-2014_12
特許番号
US08901124B2

反応ノート

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