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

Water → HCID 178437882、化合物

HRID 2257047
ノート
印刷プレビュー

反応式

HRID 2257047 の反応式
Cl.[CH2:2]([N:4]([CH2:7][C:8]1[CH:16]=[CH:15][C:11]([C:12]([OH:14])=[O:13])=[CH:10][CH:9]=1)[CH2:5][CH3:6])[CH3:3].O1CCOCC1.[CH:23]1([N:28]2[C:32]3=[N:33][C:34]([CH2:38][C:39]4[CH:44]=[CH:43][C:42](O)=[CH:41][CH:40]=4)=[N:35][C:36](=[O:37])[C:31]3=[C:30]([CH2:46][CH3:47])[NH:29]2)[CH2:27][CH2:26][CH2:25][CH2:24]1.O>C(OCC)(=O)C>[CH:23]1([N:28]2[C:32]3=[N:33][C:34]([CH2:38][C:39]4[CH:40]=[CH:41][C:42]([O:13][C:12]([C:11]5[CH:10]=[CH:9][C:8]([CH2:7][N:4]([CH2:5][CH3:6])[CH2:2][CH3:3])=[CH:16][CH:15]=5)=[O:14])=[CH:43][CH:44]=4)=[N:35][C:36](=[O:37])[C:31]3=[C:30]([CH2:46][CH3:47])[NH:29]2)[CH2:24][CH2:25][CH2:26][CH2:27]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 962WaterHCID 312751,4-Dioxane2 回HCID 122990074-((Diethylamino)methyl)benzoic acid hydrochlorideHCID 178437877HCID 178437877、化合物

生成物 1

HCID 178437882HCID 178437882、化合物収率 58.1%

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

A mixture of 4-diethylaminomethyl benzoic acid hydrochloride (360 mg, 1.5 mmol), N,N'-carbonyldiimidazole (264 mg, 1.5 mmol) and dioxane (20 ml) was heated on an oil bath for 1 hour. The reaction mixture was cooled to room temperature and 1-cyclopentyl-3-ethyl-6-(4-hydroxyphenylmethyl)pyrazolo[3,4-d]pyrimidin-4-one (500 mg, 105 mmol) and dioxane (10 ml) were added and the reaction mixture was heated at 100° C. overnight. The reaction mixture was cooled, the solvent was stripped and then water and ethyl acetate were added. The ethyl acetate layer was separated, then washed with 2N HCl (4×150 ml). The aqueous layers were combined, treated with concentrated NH4OH and then extracted with ethyl acetate (2×). The ethyl acetate layer was washed with brine, dried over MgSO4, filtered and stripped to afford crude product. The crude product was combined with the crude product from a similar experimental run and the mixture was recrystallized from ether to afford 0.46 g of 1-cyclopentyl-3-ethyl-6-[4-[4-(diethylaminomethyl)phenylcarbonyloxy]phenylmethyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 143°-145° C.

後処理

  1. temperaturewas heated on an oil bath for 1 hour
  2. temperaturethe reaction mixture was heated at 100° C. overnight
  3. temperatureThe reaction mixture was cooled
  4. customThe ethyl acetate layer was separated
  5. washwashed with 2N HCl (4×150 ml)
  6. additiontreated with concentrated NH4OH
  7. extractionextracted with ethyl acetate (2×)
  8. washThe ethyl acetate layer was washed with brine
  9. dry with materialdried over MgSO4
  10. filtrationfiltered
  11. customto afford crude product
  12. customthe mixture was recrystallized from ether

出典と根拠

ORDレコード
ord-be35d3c4b26f45ec8707790a0d712094
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05656629

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