Ammonia → HCID 86689764, 화합물

HRID 1396414노트

반응식

HRID 1396414 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 86689764HCID 86689764, 화합물수율 75%

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-6e6d937eded14545be4ce2503a8766bb
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901124B2

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