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Acetic Acid → HCID 178472505、化合物

HRID 931245
ノート
印刷プレビュー

反応式

HRID 931245 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[CH2:14][CH2:13][CH2:12][C@@H:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:10]2)=[N:6][C:7]=1[NH2:8].[CH:20]1([C:23]2[N:28]=[C:27]([CH:29]=O)[CH:26]=[CH:25][CH:24]=2)[CH2:22][CH2:21]1.[S].C(O)(=O)C>C(O)C>[CH:20]1([C:23]2[N:28]=[C:27]([C:29]3[NH:8][C:7]4=[N:6][C:5]([N:9]5[CH2:14][CH2:13][CH2:12][C@@H:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:10]5)=[CH:4][CH:3]=[C:2]4[N:1]=3)[CH:26]=[CH:25][CH:24]=2)[CH2:22][CH2:21]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 5362487SulfurHCID 193617216-CyclopropylpicolinaldehydeHCID 131735159(R)-ethyl 1-(5,6-diaminopyridin-2-yl)piperidine-3-carboxylate

生成物 1

HCID 178472505HCID 178472505、化合物収率 67%

試薬・触媒・溶媒 1

HCID 702Ethanol
溶媒

反応条件

温度
80 °C

実験手順

To a solution of (R)-ethyl 1-(5,6-diaminopyridin-2-yl)piperidine-3-carboxylate (250 mg, 0.686 mmol) in ethanol (15 mL) was added 6-cyclopropylpicolinaldehyde (55 mg, 0.823 mmol), sulfur (43 mg, 1.372 mmol) and acetic acid (1.5 mL) at room temperature. The reaction mixture was stirred at 80° C. for 18 h. The reaction mixture was poured into ice water and extracted with ethyl acetate. The organics were concentrated under reduced pressure and the crude material was purified via preparative TLC (80% ethyl acetate in petroleum ether) to afford (R)-ethyl 1-(2-(6-cyclopropylpyridin-2-yl)-3H-imidazo[4,5-b]pyridin-5-yl)piperidine-3-carboxylate (180 mg). MS (ES+APCI) (M+H) 392.2; LCMS retention time 3.757 min (Method J).

後処理

  1. extractionextracted with ethyl acetate
  2. concentrationThe organics were concentrated under reduced pressure
  3. customthe crude material was purified via preparative TLC (80% ethyl acetate in petroleum ether)

出典と根拠

ORDレコード
ord-f4f0b2bb5dff4230a1bfd575a7214a30
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296745B2

反応ノート

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