Pyridine → HCID 86601132、化合物

HRID 1916694ノート

反応式

HRID 1916694 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:14]=[CH:15][C:16]([C:19]#[C:20][C:21]3[CH:30]=[CH:29][C:24]([O:25][CH2:26][CH2:27][OH:28])=[CH:23][CH:22]=3)=[N:17][CH:18]=2)=[CH:9][CH:8]=1.C(N(CC)CC)C.N1C=CC=CC=1>C1COCC1.O>[CH3:1][S:2]([O:28][CH2:27][CH2:26][O:25][C:24]1[CH:23]=[CH:22][C:21]([C:20]#[C:19][C:16]2[CH:15]=[CH:14][C:13]([C:10]3[CH:9]=[CH:8][C:7]([Cl:6])=[CH:12][CH:11]=3)=[CH:18][N:17]=2)=[CH:30][CH:29]=1)(=[O:4])=[O:3]

参加物

7

反応物 4

HCID 1049PyridineHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 67363953HCID 67363953、化合物

生成物 1

HCID 86601132HCID 86601132、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

0.59 mL (7.55 mmol) methanesulphonic acid chloride are added dropwise to a solution, cooled to 0° C., of 2.2 g (6.29 mmol) 2-{4-[5-(4-chloro-phenyl)-pyridin-2-ylethynyl]-phenoxy}-ethanol and 1.74 mL (12.58 mmol) triethylamine in 25 mL THF. The reaction mixture is heated to RT and stirred for 2 h. To complete the reaction 5 mL pyridine are added and kept at RT for a further 18 h. The solvent is eliminated i.vac., the residue is combined with water and triturated with diethyl ether. The product precipitated is suction filtered and dried.

後処理

  1. additionare added
  2. waitkept at RT for a further 18 h
  3. customtriturated with diethyl ether
  4. customThe product precipitated
  5. filtrationfiltered
  6. customdried

出典と根拠

ORDレコード
ord-fc63fe49e1fa45b091552ad0eaf676e8
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

反応ノート

読み込み中…