ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

4-Methylmorpholine → 1-[4-(2-Carbamoylpyridin-4-yloxy)-2-fluorophenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester

HRID 409932
ノート
印刷プレビュー

反応式

HRID 409932 の反応式
S(Cl)(Cl)=O.[CH2:5]([O:12][C:13]([C:15]1([C:18]([OH:20])=O)[CH2:17][CH2:16]1)=[O:14])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[NH2:21][C:22]1[CH:38]=[CH:37][C:25]([O:26][C:27]2C=CN=C(CC(N)=O)[CH:28]=2)=[CH:24][C:23]=1[F:39].C[N:41]1[CH2:46][CH2:45][O:44][CH2:43][CH2:42]1.C[N:48]1CCCC1=O>O1CCCC1.O>[CH2:5]([O:12][C:13]([C:15]1([C:18](=[O:20])[NH:21][C:22]2[CH:38]=[CH:37][C:25]([O:26][C:27]3[CH:43]=[CH:42][N:41]=[C:46]([C:45](=[O:44])[NH2:48])[CH:28]=3)=[CH:24][C:23]=2[F:39])[CH2:16][CH2:17]1)=[O:14])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 79724-MethylmorpholineHCID 13387N-methyl-2-pyrrolidone2 回HCID 24386Thionyl ChlorideHCID 574708601-((Benzyloxy)carbonyl)cyclopropanecarboxylic acidHCID 1317316354-(4-Amino-3-fluorophenoxy)pyridine-2-carboxyamide

生成物 1

HCID 24788499
1-[4-(2-Carbamoylpyridin-4-yloxy)-2-fluorophenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Thionyl chloride was added at −20° C. to a solution of 1-(benzyloxycarbonyl)cyclopropanecarboxylic acid (97.98 g) in tetrahydrofuran (200 ml) and N-methylpyrrolidone (200 ml) and stirred for 30 minutes. A solution of 4-(4-amino-3-fluorophenoxy)pyridine-2-carboxyamide (100 g) and N-methylmorpholine (40.91 g) in N-methylpyrrolidone (600 ml) were added to the reaction mixture at the same temperature and stirred for 1 hour at 10° C. Water (100 g) was added to the reaction mixture and stirred for 1 hour at 20° C. After confirming the crystal precipitation, a 1N sodium hydroxide aqueous solution (1 L) was added and further stirred for 19 hours. The precipitated solid was collected by filtration and washed with water (500 g). The obtained solid was dried for 20 hours at 60° C. to give 176.7 g of the title compound.

後処理

  1. stirringstirred for 1 hour at 10° C
  2. stirringstirred for 1 hour at 20° C
  3. customthe crystal precipitation
  4. additiona 1N sodium hydroxide aqueous solution (1 L) was added
  5. stirringfurther stirred for 19 hours
  6. filtrationThe precipitated solid was collected by filtration
  7. washwashed with water (500 g)
  8. customThe obtained solid was dried for 20 hours at 60° C.

出典と根拠

ORDレコード
ord-f5229ec57e0440a398aace9b2b83cb4b
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08759530B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート