Hydrochloric Acid → HCID 16747649、化合物

HRID 1928374

反応式

HRID 1928374 の反応式
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

参加物

7

反応物 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

生成物 1

HCID 16747649HCID 16747649、化合物収率 81%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 10311-Propanol溶媒

実験手順

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)−].

後処理

  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

出典と根拠

ORDレコード
ord-67c53f26fef24286a54bf2b971a17083
出典データセット
uspto-grants-2012_05
特許番号
US08183262B2

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