1,3-Propanediamine → HCID 10164511、化合物

HRID 1373838ノート

反応式

HRID 1373838 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:23]([C:24]3[CH:29]=[CH:28][N:27]=[C:26](F)[CH:25]=3)=[C:11]3[CH:12]=[CH:13][CH:14]=[C:15]([C:16]4[CH:21]=[CH:20][N:19]=[C:18](F)[CH:17]=4)[N:10]3[N:9]=2)=[CH:4][CH:3]=1.[NH2:31][CH2:32][CH2:33][CH2:34][NH2:35]>>[NH2:31][CH2:32][CH2:33][CH2:34][NH:35][C:26]1[CH:25]=[C:24]([C:23]2[C:8]([C:5]3[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=3)=[N:9][N:10]3[C:15]([C:16]4[CH:21]=[CH:20][N:19]=[C:18]([NH:9][CH2:8][CH2:23][CH2:11][NH2:10])[CH:17]=4)=[CH:14][CH:13]=[CH:12][C:11]=23)[CH:29]=[CH:28][N:27]=1

参加物

3

反応物 2

HCID 4281,3-PropanediamineHCID 10157930HCID 10157930、化合物

生成物 1

HCID 10164511HCID 10164511、化合物収率 46%

実験手順

A solution of 2-(4-fluorophenyl)-3,7-bis(2-fluoropyridin-4-yl)pyrazolo[1,5-α]pyridine (34 mg, 0.08 mmol) in 1,3-diaminopropane (1 mL) was heated at 150° C. for 0.25 hours. Upon cooling to room temperature, the mixture was concentrated in vacuo and the residue was triturated with hot ethyl acetate. The resulting solids were collected on filter, washed with ethyl ether and dried to provide N-{4-[3-{2-[(3-aminopropyl)amino]pyridin-4-yl}-2-(4-fluorophenyl)pyrazolo[1,5-α]pyridin-7-yl]pyridin-2-yl}propane-1,3-diamine as a light yellow powder (19 mg, 46%). 1H NMR (CD3OD): δ 8.18 (d, 1H), 8.03 (d, 1H), 7.78 (d, 1H), 7.65 (dd, 2H), 7.45 (dd, 1H), 7.30 (s, 1H), 7.1–7.2 (m, 4H), 6.60 (s, 1H), 6.59 (d, 1H), 3.55 (t, 2H), 3.47 (t, 2H), 3.0 (q, 4H), 1.88–2.04 (m, 4H); MS m/z 511 (M+1).

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. customthe residue was triturated with hot ethyl acetate
  3. customThe resulting solids were collected
  4. filtrationon filter
  5. washwashed with ethyl ether
  6. customdried

出典と根拠

ORDレコード
ord-20ecc05d187d4db890cf0dcba5183a6c
出典データセット
uspto-grants-2007_01
特許番号
US07163940B2

反応ノート

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