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Triethylamine → HCID 178434276、化合物

HRID 711110
ノート
印刷プレビュー

反応式

HRID 711110 の反応式
Cl.[CH:2]([N:5]1[C:9]2[C:10](=[O:19])[NH:11][C:12]3([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[CH2:13][C:8]=2[CH:7]=[N:6]1)([CH3:4])[CH3:3].[CH3:20][C:21]1[C:29]2[C:24](=[C:25]([CH3:33])[CH:26]=[C:27]([C:30](O)=[O:31])[CH:28]=2)[NH:23][N:22]=1.C(N(CC)CC)C.CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>CN(C)C=O.CN(C)C1C=CN=CC=1.C(OCC)(=O)C>[CH3:20][C:21]1[C:29]2[C:24](=[C:25]([CH3:33])[CH:26]=[C:27]([C:30]([N:16]3[CH2:17][CH2:18][C:12]4([NH:11][C:10](=[O:19])[C:9]5[N:5]([CH:2]([CH3:4])[CH3:3])[N:6]=[CH:7][C:8]=5[CH2:13]4)[CH2:14][CH2:15]3)=[O:31])[CH:28]=2)[NH:23][N:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 111923Propylphosphonic anhydrideHCID 674915351'-Isopropyl-4',6'-dihydrospiro[piperidine-4,5'-pyrazolo[3,4-c]pyridin]-7'(1'H)-one hydrochloride2 回HCID 178434277HCID 178434277、化合物

生成物 1

HCID 178434276HCID 178434276、化合物収率 25.2%

試薬・触媒・溶媒 3

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1′-isopropyl-4′,6′-dihydrospiro[piperidine-4,5′-pyrazolo[3,4-c]pyridin]-7′(1′H)-one hydrochloride salt (Intermediate 2, 430 mg, 1.3 mmol) and 3,7-dimethyl-1H-indazole-5-carboxylic acid (306 mg, 1.6 mmol) in dimethylformamide (2 mL) was added triethylamine (0.75 mL, 5.4 mmol), 4-dimethylaminopyridine (33 mg, 0.37 mmol), and 1-propanephosphonic acid cyclic anhydride (0.52 mL, 1.74 mmol, 50% solution in ethyl acetate), and the reaction mixture was stirred overnight at room temperature. The reaction mixture was concentrated in vacuo, taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate. The organic layer was dried over sodium sulfate, filtered, and concentrated to a solid. The solid was purified via flash column chromatography (0-15% methanol/dichloromethane) to afford a glassy solid. The glassy solid was stirred in ethyl acetate for 16 hours and the resulting solid collected by vacuum filtration to afford the desired product as a white solid (138 mg). +ESI (M+H) 421.0; 1H NMR (400 MHz, CD3OD, δ): 7.65 (s, 1H) 7.42 (s, 1H) 7.21 (s, 1H) 5.50 (m, 1H) 3.95 (br. s., 1H) 3.50-3.62 (br. s., 3H) 2.97 (s, 2H) 2.56 (m, 6H) 1.83 (br. s., 4H) 1.44 (d, 6H).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. washwashed with saturated aqueous sodium bicarbonate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to a solid
  6. customThe solid was purified via flash column chromatography (0-15% methanol/dichloromethane)
  7. customto afford a glassy solid
  8. filtrationthe resulting solid collected by vacuum filtration

出典と根拠

ORDレコード
ord-c302c3b6c384424cb089e0e9977b7602
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181252B2

反応ノート

読み込み中…

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