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

Methyl Isobutyl Ketone → HCID 20385629、化合物

HRID 1704517
ノート
印刷プレビュー

反応式

HRID 1704517 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[N:6]([CH:10]3[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[C:7](=[O:9])[NH:8][C:4]=2[CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].CC(C)CC(=O)C.Br[CH2:32][CH2:33][CH2:34][N:35]1[C:39]2[CH:40]=[CH:41][CH:42]=[CH:43][C:38]=2[N:37]=[N:36]1>O>[N:35]1([CH2:34][CH2:33][CH2:32][N:13]2[CH2:12][CH2:11][CH:10]([N:6]3[C:5]4[CH:16]=[CH:17][C:2]([Cl:1])=[CH:3][C:4]=4[NH:8][C:7]3=[O:9])[CH2:15][CH2:14]2)[C:39]2[CH:40]=[CH:41][CH:42]=[CH:43][C:38]=2[N:37]=[N:36]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7909Methyl Isobutyl KetoneHCID 10340Sodium CarbonateHCID 1046075-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 3732348HCID 3732348、化合物

生成物 1

HCID 20385629HCID 20385629、化合物収率 25%

試薬・触媒・溶媒 1

HCID 962Water
溶媒
2 回

実験手順

A mixture of 5 parts of 5-chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 3.7 parts of sodium carbonate and 200 parts of 4-methyl-2-pentanone is stirred and refluxed with water-separator. Then there are added 4.8 parts of 1-(3-bromopropyl)-1H-benzotriazole and stirring is continued overnight at reflux temperature. The reaction mixture is cooled, water is added and the undissolved product is filtered off and set aside. The organic phase is separated from the filtrate, dried, filtered and evaporated. The residue is combined with the undissolved product (see above) and purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone, yielding 2 parts (25%) of 1-{1-[3-(1H-benzotriazol-1-yl)propyl]-4-piperidinyl}-5-chloro-1,3-dihydro-2H-benzimidazol-2-one; mp. 203.4° C.

後処理

  1. stirringstirring
  2. temperatureat reflux temperature
  3. temperatureThe reaction mixture is cooled
  4. filtrationthe undissolved product is filtered off
  5. customThe organic phase is separated from the filtrate
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. custompurified by column-chromatography over silica gel using
  10. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
  11. customThe pure fractions are collected
  12. customthe eluent is evaporated
  13. customThe residue is crystallized from 4-methyl-2-pentanone

出典と根拠

ORDレコード
ord-a76323dcaaff4c238081c1470fba6736
出典データセット
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04126687

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