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Triethylamine → Cyclopropanesulfonic acid N-{1-[2-methoxypyridin-4-yl]-1-[(1-pyridin-3-yl-1H-indazol-5-yl)oxy]propan-2-yl}amide

HRID 1661483
ノート
印刷プレビュー

反応式

HRID 1661483 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH:9]([O:13][C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[N:19]([C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[N:18]=[CH:17]3)[CH:10]([NH2:12])[CH3:11])[CH:6]=[CH:5][N:4]=1.C(N(CC)CC)C.[CH:36]1([S:39](Cl)(=[O:41])=[O:40])[CH2:38][CH2:37]1.[NH4+].[Cl-]>ClCCl.CN(C1C=CN=CC=1)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH:9]([O:13][C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[N:19]([C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[N:18]=[CH:17]3)[CH:10]([NH:12][S:39]([CH:36]2[CH2:38][CH2:37]2)(=[O:41])=[O:40])[CH3:11])[CH:6]=[CH:5][N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 2760919Cyclopropanesulfonyl chlorideHCID 597865661-[2-Methoxypyridin-4-yl]-1-[1-(pyridin-3-yl)indazol-5-yl]oxypropan-2-amine

生成物 1

HCID 59786581Cyclopropanesulfonic acid N-{1-[2-methoxypyridin-4-yl]-1-[(1-pyridin-3-yl-1H-indazol-5-yl)oxy]propan-2-yl}amide

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 1-[2-methoxypyridin-4-yl]-1-[1-(pyridin-3-yl)indazol-5-yl]oxypropan-2-amine (41 mg, 110 μmol) in dichloromethane (4 ml) was added triethylamine (36 μl), followed by cyclopropanesulfonic acid chloride (23 mg, i 60 μmol) and DMAP (1.3 mg, 11 μmol).The stirring was continued for 20 h at room temp. The reaction mixture was poured into sat. NH4Cl solution and extracted with dichloromethane then the solvent was removed i.vac., and the product purified by chromatography on silica gel. Yield 4 mg (7.6%) as a racemic mixture of one diastereomer.

後処理

  1. extractionextracted with dichloromethane
  2. customthe solvent was removed i.vac
  3. custom, and the product purified by chromatography on silica gel
  4. additionYield 4 mg (7.6%) as a racemic mixture of one diastereomer

出典と根拠

ORDレコード
ord-e40fad2826e64b549655929df9917da6
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030340B2

反応ノート

読み込み中…

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