Hydrochloric Acid → HCID 16747649, 화합물

HRID 1928374

반응식

HRID 1928374 반응식
CC(C)(C)C[O:4][S:5]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([C:14]2[N:19]=[C:18]([C:20]3[CH:25]=[C:24]([C:26]4[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:28][CH:27]=4)[CH:23]=[C:22]([CH3:36])[N:21]=3)[CH:17]=[CH:16][CH:15]=2)[CH:9]=1)(=[O:7])=[O:6].C([O-])CC.[Na+].C(N(CC)CCS)C.Cl>C(O)CC.O>[CH3:36][C:22]1[N:21]=[C:20]([C:18]2[CH:17]=[CH:16][CH:15]=[C:14]([C:10]3[CH:9]=[C:8]([S:5]([OH:7])(=[O:4])=[O:6])[CH:13]=[CH:12][CH:11]=3)[N:19]=2)[CH:25]=[C:24]([C:26]2[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:33])[F:34])=[CH:28][CH:27]=2)[CH:23]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 160322-(Diethylamino)ethanethiolHCID 236693631-Propanol, sodium salt (1:1)HCID 866154673-[6'-Methyl-4'-(4-trifluoromethyl-phenyl)-[2,2']bipyridinyl-6-yl]-benzenesulfonic acid 2,2-dimethyl-propyl ester

생성물 1

HCID 16747649HCID 16747649, 화합물수율 81%

시약·촉매·용매 2

HCID 962Water용매HCID 10311-Propanol용매

실험 절차

The title compound was prepared from the above described 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonic acid 2,2-dimethyl-propyl ester (7.7 g, 14.24 mmol) by refluxing in 1-propanol (15 mL) with sodium propanolate (1.7 M in n-propanol, 20.95 ml, 35.6 mmol) and 2-(diethylamino)ethanthiol (2.48 mL, 16.38 mmol) for 18 h. Cooled to rt, added water (300 mL), added 1 N HCl (ca. 50 mL) until pH 3-4 was reached, stirred for 10 min, filtered the solid off, washed thrice with water, and then with acetone and dried in HV to give the title compound (5.4 g, 81%) as an off-white solid. MS (ISN) 469.1 [(M−H)−].

후처리

  1. customThe title compound was prepared from the
  2. filtrationfiltered the solid off,
  3. washwashed thrice with water
  4. dry with materialwith acetone and dried in HV

출처 및 근거

ORD 기록
ord-67c53f26fef24286a54bf2b971a17083
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183262B2

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