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Periodate → 1-(6-{[6-(4-Fluorophenyl)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]sulphanyl}-1,3-benzothiazol-2-yl)-3-[2-(4-oxidomorpholin-4-yl)ethyl]urea

HRID 1035777
ノート
印刷プレビュー

反応式

HRID 1035777 の反応式
I([O-])(=O)(=O)=O.[Na].[F:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:15]=[CH:16][C:17]3[N:18]([C:20]([S:23][C:24]4[CH:44]=[CH:43][C:27]5[N:28]=[C:29]([NH:31][C:32]([NH:34][CH2:35][CH2:36][N:37]6[CH2:42][CH2:41][O:40][CH2:39][CH2:38]6)=[O:33])[S:30][C:26]=5[CH:25]=4)=[N:21][N:22]=3)[N:19]=2)=[CH:10][CH:9]=1.I([O-])(=O)(=O)=[O:46].[Na+]>O.C(O)(=O)C>[F:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:15]=[CH:16][C:17]3[N:18]([C:20]([S:23][C:24]4[CH:44]=[CH:43][C:27]5[N:28]=[C:29]([NH:31][C:32]([NH:34][CH2:35][CH2:36][N+:37]6([O-:46])[CH2:42][CH2:41][O:40][CH2:39][CH2:38]6)=[O:33])[S:30][C:26]=5[CH:25]=4)=[N:21][N:22]=3)[N:19]=2)=[CH:10][CH:9]=1
参加物反応条件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 167232PeriodateHCID 5360545SodiumHCID 23667635Sodium periodateHCID 25182860Sar-125844

生成物 1

HCID 867620901-(6-{[6-(4-Fluorophenyl)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]sulphanyl}-1,3-benzothiazol-2-yl)-3-[2-(4-oxidomorpholin-4-yl)ethyl]urea収率 75.3%

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
2 回
HCID 962Water溶媒2 回

反応条件

温度
20 °C

実験手順

116 mg of periodate of sodium in 0.5 cm3 of water are added to a mixture of 200 mg of 1-(6-{[6-(4-fluorophenyl)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]sulphanyl}-1,3-benzothiazol-2-yl)-3-[2-(morpholin-4-yl)ethyl]urea in 5 cm3 of acetic acid at 20° C. After an overnight period, the precipitate is filtered off. The white powder obtained is a mixture containing oxidized product and starting product. This mixture is taken up in 10 cm3 of acetic acid with 155 mg of sodium periodate dissolved in 1 cm3 of water. The mixture is left to stir overnight at 20° C. The precipitate is then filtered off and then washed successively with diisopropyl ether and with diethyl ether. 155 mg of white powder of 1-(6-{[6-(4-fluorophenyl)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]sulphanyl}-1,3-benzothiazol-2-yl)-3-[2-(4-oxidomorpholin-4-yl)ethyl]urea are obtained, the characteristics of which are as follows:

後処理

  1. filtrationthe precipitate is filtered off
  2. customThe white powder obtained
  3. additioncontaining oxidized product
  4. waitThe mixture is left
  5. filtrationThe precipitate is then filtered off
  6. washwashed successively with diisopropyl ether and with diethyl ether

出典と根拠

ORDレコード
ord-9c9d0ad901df40f195f65aec9915434c
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546393B2

反応ノート

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