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

Lithium Hydroxide → HCID 68793468、化合物

HRID 1784309
ノート
印刷プレビュー

反応式

HRID 1784309 の反応式
[OH-].[Li+].[CH3:3][CH:4]([CH3:46])[CH2:5][CH2:6][N:7]([CH2:41][CH2:42][CH:43]([CH3:45])[CH3:44])[C:8]([C:10]1[CH:11]=[CH:12][C:13]2[N:17]=[C:16]([NH:18][C:19]3[CH:28]=[CH:27][C:22]([C:23]([O:25]C)=[O:24])=[CH:21][CH:20]=3)[N:15]([CH2:29][CH2:30][CH2:31][NH:32][C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[C:14]=2[CH:40]=1)=[O:9]>O1CCCC1.O.C(OCC)C>[CH3:44][CH:43]([CH3:45])[CH2:42][CH2:41][N:7]([CH2:6][CH2:5][CH:4]([CH3:46])[CH3:3])[C:8]([C:10]1[CH:11]=[CH:12][C:13]2[N:17]=[C:16]([NH:18][C:19]3[CH:28]=[CH:27][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=3)[N:15]([CH2:29][CH2:30][CH2:31][NH:32][C:33]([O:35][C:36]([CH3:39])([CH3:37])[CH3:38])=[O:34])[C:14]=2[CH:40]=1)=[O:9]
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 2

HCID 3939Lithium HydroxideHCID 68792031methyl 4-[(6-{[bis(3-methylbutyl)amino]carbonyl}-1-{3-[(tert-butoxycarbonyl) amino]propyl}-1H-benzimidazol-2-yl)amino]benzoate

生成物 1

HCID 68793468HCID 68793468、化合物収率 79%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

Lithium hydroxide (141 mg, 5 eq) is added to methyl 4-[(6-{[bis(3-methylbutyl)amino]carbonyl}-1-{3-[(tert-butoxycarbonyl)amino]propyl}-1H-benzimidazol-2-yl)amino]benzoate prepared according to reaction diagram A, Example A1, (405 mg, 1 eq) in a mixture of tetrahydrofuran (4 ml) and water (3 ml). The mixture is heated under reflux for 18 hours then cooled down to ambient temperature and concentrated under reduced pressure at 40° C. Dichloromethane (50 ml) and water (20 ml) are added to the residue. The mixture is acidified by the addition of acetic acid to pH 5. After decantation and extractions, the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. The solid obtained is taken up in ethyl ether in order to produce the expected compound (309 mg; 79%).

後処理

  1. customprepared
  2. customaccording to reaction diagram A, Example A1, (405 mg, 1 eq)
  3. temperatureThe mixture is heated
  4. temperatureunder reflux for 18 hours
  5. concentrationconcentrated under reduced pressure at 40° C
  6. additionDichloromethane (50 ml) and water (20 ml) are added to the residue
  7. additionThe mixture is acidified by the addition of acetic acid to pH 5
  8. extractionAfter decantation and extractions
  9. dry with materialthe combined organic phases are dried over sodium sulphate
  10. concentrationconcentrated under reduced pressure
  11. customThe solid obtained

出典と根拠

ORDレコード
ord-ff5fd7c600514d0a90e36840d81a472a
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07501525B2

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