Pyridine → HCID 86601132, 화합물

HRID 1916694노트

반응식

HRID 1916694 반응식
[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]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 67363953HCID 67363953, 화합물

생성물 1

HCID 86601132HCID 86601132, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fc63fe49e1fa45b091552ad0eaf676e8
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618132B2

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