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

p-Toluenesulfonic acid monohydrate → 3-ethoxy-4-[(6-methyl-5-oxo-2-propan-2-yl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-10-yl)amino]-N-[(3R)-1-methylpyrrolidin-3-yl]benzamide

HRID 2234304
ノート
印刷プレビュー

反応式

HRID 2234304 の反応式
Cl[C:2]1[N:12]=[C:11]2[C:5]([N:6]([CH3:17])[C:7](=[O:16])[CH2:8][CH2:9][N:10]2[CH:13]([CH3:15])[CH3:14])=[CH:4][N:3]=1.[NH2:18][C:19]1[CH:33]=[CH:32][C:22]([C:23]([NH:25][C@@H:26]2[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27]2)=[O:24])=[CH:21][C:20]=1[O:34][CH2:35][CH3:36].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)CC(O)C>[CH2:35]([O:34][C:20]1[CH:21]=[C:22]([CH:32]=[CH:33][C:19]=1[NH:18][C:2]1[N:12]=[C:11]2[C:5]([N:6]([CH3:17])[C:7](=[O:16])[CH2:8][CH2:9][N:10]2[CH:13]([CH3:15])[CH3:14])=[CH:4][N:3]=1)[C:23]([NH:25][C@@H:26]1[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27]1)=[O:24])[CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 521998p-Toluenesulfonic acid monohydrateHCID 686812194-amino-3-ethoxy-N-[(3R)-1-methylpyrrolidin-3-yl]benzamide2 回HCID 866175432-Chloro-9-isopropyl-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one2 回

生成物 1

HCID 686815373-ethoxy-4-[(6-methyl-5-oxo-2-propan-2-yl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-10-yl)amino]-N-[(3R)-1-methylpyrrolidin-3-yl]benzamide収率 61%

試薬・触媒・溶媒 1

HCID 79104-Methyl-2-Pentanol溶媒

実験手順

10-Chloro-6-methyl-2-propan-2-yl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-5-one (Intermediate 10; 100 mg, 0.39 mmol), 4-amino-3-ethoxy-N-[(3R)-1-methylpyrrolidin-3-yl]benzamide (Intermediate 166; 104 mg, 0.39 mmol) and 4-toluenesulphonic acid monohydrate (187 mg, 0.98 mmol) were heated in 4-methyl-2-pentanol (3 mL) at 140° C. for 3 hours. The cooled reaction mixture was absorbed on to an SCX column, washed with methanol and eluted with ammonia in methanol. Product containing fractions were concentrated and purified by base modified preparative reverse phase HPLC to yield the title compound as a white solid (114 mg, 61%).

後処理

  1. customThe cooled reaction mixture
  2. customwas absorbed on to an SCX column
  3. washwashed with methanol
  4. washeluted with ammonia in methanol
  5. additionProduct containing fractions
  6. concentrationwere concentrated
  7. custompurified by base

出典と根拠

ORDレコード
ord-336ac97d9b6e4c63b56f60294738c84e
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709471B2

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