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

Ethanol → (R)-3-[N-(5'-Chloro-2'-fluorobiphenyl-4-ylmethyl)-N'-(2-hydroxythiazole-5-carbonyl)hydrazino]-2-hydroxypropionic Acid

HRID 541505
ノート
印刷プレビュー

反応式

HRID 541505 の反応式
[OH:1][C:2]1[S:3][C:4]([C:7]([OH:9])=O)=[CH:5][N:6]=1.CN(C(ON1N=NC2C=CC(=CC1=2)Cl)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN(C=O)C.C([O:42][C:43](=[O:64])[C@H:44]([OH:63])[CH2:45][N:46]([CH2:48][C:49]1[CH:54]=[CH:53][C:52]([C:55]2[CH:60]=[C:59]([Cl:61])[CH:58]=[CH:57][C:56]=2[F:62])=[CH:51][CH:50]=1)[NH2:47])C.CCN(C(C)C)C(C)C.CCO.[Li+].[OH-].O>>[Cl:61][C:59]1[CH:58]=[CH:57][C:56]([F:62])=[C:55]([C:52]2[CH:53]=[CH:54][C:49]([CH2:48][N:46]([CH2:45][C@@H:44]([OH:63])[C:43]([OH:64])=[O:42])[NH:47][C:7]([C:4]3[S:3][C:2]([OH:1])=[N:6][CH:5]=3)=[O:9])=[CH:50][CH:51]=2)[CH:60]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 8

HCID 702EthanolHCID 962WaterHCID 3939Lithium HydroxideHCID 6228DimethylformamideHCID 81531DiisopropylethylamineHCID 200616172-Oxo-2,3-dihydro-1,3-thiazole-5-carboxylic acidHCID 42624899O-(6-Chlorobenzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate
HCID 67972425(R)-3-[N-(5'-Chloro-2'-fluorobiphenyl-4-ylmethyl)hydrazino]-2-hydroxypropionic Acid Ethyl Ester

生成物 1

HCID 178523955(R)-3-[N-(5'-Chloro-2'-fluorobiphenyl-4-ylmethyl)-N'-(2-hydroxythiazole-5-carbonyl)hydrazino]-2-hydroxypropionic Acid収率 15.7%

実験手順

2-Hydroxy-5-thiazolecarboxylic acid (43.5 mg, 0.3 mmol) and HCTU (124 mg, 0.3 mmol) were stirred in DMF (1.3 mL, 16.4 mmol) for 15 minutes at room temperature. (R)-3-[N-(5′-Chloro-2′-fluorobiphenyl-4-ylmethyl)hydrazino]-2-hydroxypropionic acid ethyl ester (100 mg, 0.3 mmol) and DIPEA (142 μL, 818 μmol) were added, and resulting mixture was stirred at room temperature for 30 minutes. The mixture was then evaporated under reduced pressure. The residue was dissolved in EtOH (955 μL, 16.4 mmol). A solution of 1.0 M LiOH in water (1.4 mL, 1.4 mmol) was added and the resulting mixture was stirred at 40° C. for 3 hours. LC/MS showed completion. The solvent was removed in vacuo and the residue was purified by preparative HPLC to yield the title compound (22 mg) as a TFA salt. MS m/z [M+H]+ calc'd for C20H17ClFN3O5S, 466.06. found 466.0.

後処理

  1. customresulting mixture
  2. customThe mixture was then evaporated under reduced pressure
  3. stirringthe resulting mixture was stirred at 40° C. for 3 hours
  4. customThe solvent was removed in vacuo
  5. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-a2967c70a53744ca81c666d98f23919b
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871792B2

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