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

Trifluoroacetic acid → HCID 131727015、化合物

HRID 29171
ノート
印刷プレビュー

反応式

HRID 29171 の反応式
[C:1]1([CH3:10])[C:2]([C:7](Cl)=[O:8])=[CH:3][CH:4]=[CH:5][CH:6]=1.[NH2:11][C@@H:12]([CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C@H:13]([OH:33])[CH2:14][N:15](OC1CCCC1)[S:16]([C:19]1[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=1)(=[O:18])=[O:17].F[C:42](F)(F)[C:43]([OH:45])=O.[CH:48](N(CC)C(C)C)([CH3:50])[CH3:49]>ClCCl>[CH2:34]([C@H:12]([NH:11][C:7](=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[CH3:10])[C@@H:13]([OH:33])[CH:14]([NH:15][S:16]([C:19]1[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=1)(=[O:17])=[O:18])[O:45][CH:43]1[CH2:42][CH2:50][CH2:48][CH2:49]1)[C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=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 6422Trifluoroacetic acidHCID 702762-Methylbenzoyl chlorideHCID 81531DiisopropylethylamineHCID 57010648N1-[(2R,3S)-3-amino-2-hydroxy-4-phenylbutyl)-N1-(cyclopentyloxy)-4-methoxy-1-benzenesulfonamide

生成物 1

HCID 131727015HCID 131727015、化合物収率 89%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

o-Toluoyl chloride (7.8 μL, 0.0602 mmol) was added to a solution of N1-[(2R,3S)-3-amino-2-hydroxy-4-phenylbutyl]-N1-(cyclopentyloxy)-4-methoxy-1-benzenesulfonamide×trifluoracetic acid (Step 1, Example 48), (30 mg, 0.055 mmol) and N,N-diisopropylethylamine (23.8 μL, 0.137 mmol) in approximately 1.5 mL of dichloromethane under Argon. After stirring for 18 hours at ambient temperature, the reaction solvent was removed in vacuo and the residue was purified on a preparative TLC plate (20×20 cm, 500 μM) eluting with 96:4 methylene chloride:methanol. The product band was removed, eluted with 4:1 methylene chloride:methanol, filtered, and evaporated in vacuo. The residue was triturated from diethylether and hexane and the solvents were evaporated in vacuo to provide N1-((1S,2R)-1-benzyl-3-(cyclopentyloxy)[(4-methoxyphenyl)sulfonyl]amino-2-hydroxypropyl)-2-methylbenzamide (27 mg, 89%) as a solid. H1-NMR (dimethylsulfoxide-D6): 1.75 (m, 8H), 1.87 (s, 3H), 2.63 (m, 1H), 2.79 (bm, 1H), 3.05 (bm, 1H), 3.21 (bm, 1H), 3.69 (bm, 1H), 3.86 (s, 3H), 4.13 (bm, 1H), 4.86 (bm, 1H), 5.28 (bs, 1H), 6.79 (m, 1H), 7.21 (m, 10H), 7.72 (d, 2H), 8.06 (d, 1H). MS(ESI): 575(M+Na).

後処理

  1. customthe reaction solvent was removed in vacuo
  2. customthe residue was purified on a preparative TLC plate (20×20 cm, 500 μM)
  3. washeluting with 96:4 methylene chloride
  4. customThe product band was removed
  5. washeluted with 4:1 methylene chloride
  6. filtrationmethanol, filtered
  7. customevaporated in vacuo
  8. customThe residue was triturated from diethylether and hexane
  9. customthe solvents were evaporated in vacuo

出典と根拠

ORDレコード
ord-d950ddd320ca4e63a25573cca25af9f8
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07419967B2

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