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Acetic Acid → HCID 178489609、化合物

HRID 1871593
ノート
印刷プレビュー

反応式

HRID 1871593 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([C:14]#[N:15])[CH:9]=2)[N:5]=[C:4]([NH:16][S:17]([C:20]2[CH:25]=[CH:24][C:23]([CH:26]([CH3:28])[CH3:27])=[CH:22][N:21]=2)(=[O:19])=[O:18])[C:3]=1[O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[O:36][CH3:37].O.[NH2:39][NH2:40].C(O)(=O)C>CN(C)C=O.O>[Cl:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([C:14]([NH:39][NH2:40])=[NH:15])[CH:9]=2)[N:5]=[C:4]([NH:16][S:17]([C:20]2[CH:25]=[CH:24][C:23]([CH:26]([CH3:28])[CH3:27])=[CH:22][N:21]=2)(=[O:19])=[O:18])[C:3]=1[O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[O:36][CH3:37]
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

6

反応物 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 54403314N-(6-chloro-2-(2-cyanopyridin-4-yl)-5-(2-methoxyphenoxy)pyrimidin-4-yl)-5-isopropylpyridine-2-sulfonamide

生成物 1

HCID 178489609HCID 178489609、化合物収率 97%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
15 °C

実験手順

122 g (233 mmol) of 5-isopropyl-pyridine-2-sulfonic acid [6-chloro-2-(2-cyano-pyridine-4-yl)-5-(2-methoxy-phenoxy)-pyrimidine-4-yl]-amide was suspended in 450 ml of N,N-dimethyl formamide and the mixture was cooled down to 15° C. At this temperature, 35 ml of hydrazine hydrate were added dropwise within 1 hr. The resulting solution was stirred at 15° C. to 20° C. for 16 hr and thereafter diluted with 600 ml of de-ionized water. Then 50 ml of glacial acetic acid were added dropwise at 0° C. to 5° C. until pH=5.5. 600 g of ice were added and the suspension was stirred for 1 hr. The solid was filtered off under suction, washed with 3000 ml of water and dried at 40° C., 2000 Pa for 24 hr. There were obtained 126 g (97% of theory) of 5-isopropyl-pyridine-2-sulfonic acid [6-chloro-2-[2-(hydrazino-imino-methyl)-pyridine-4-yl]-5-(2-methoxy-phenoxy)-pyrimidine-4-yl]-amide with a HPLC purity of 91.8% (w/w).

後処理

  1. stirringthe suspension was stirred for 1 hr
  2. filtrationThe solid was filtered off under suction
  3. washwashed with 3000 ml of water
  4. customdried at 40° C.
  5. wait2000 Pa for 24 hr

出典と根拠

ORDレコード
ord-8871e54a1fc0444ca845540299ea3a95
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06103902

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート