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Acetic Acid → HCID 86705124、化合物

HRID 541551
ノート
印刷プレビュー

反応式

HRID 541551 の反応式
[C:1](=[O:8])([O:5][CH2:6][CH3:7])[O:2][CH2:3]Cl.[Na+].[I-].O=C(C1C=CC=CC=1)C[O:14][C:15](=[O:43])[C@H:16]([OH:42])[CH2:17][N:18]([CH2:28][C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([Cl:41])[CH:36]=2)=[CH:31][CH:30]=1)[NH:19][C:20]([C:22]1[O:26][N:25]=[C:24]([OH:27])[CH:23]=1)=[O:21].C(=O)([O-])[O-].[Cs+].[Cs+].CC(O)=O>CC(C)=O.[Zn]>[Cl:41][C:37]1[CH:36]=[C:35]([C:32]2[CH:31]=[CH:30][C:29]([CH2:28][N:18]([CH2:17][C@@H:16]([OH:42])[C:15]([OH:43])=[O:14])[NH:19][C:20]([C:22]3[O:26][N:25]=[C:24]([O:27][CH2:3][O:2][C:1]([O:5][CH2:6][CH3:7])=[O:8])[CH:23]=3)=[O:21])=[CH:34][CH:33]=2)[CH:40]=[CH:39][CH:38]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 176Acetic AcidHCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 5325479Chloromethyl Ethyl CarbonateHCID 178521475HCID 178521475、化合物

生成物 1

HCID 86705124HCID 86705124、化合物収率 7.6%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒
HCID 180Acetone溶媒2 回

反応条件

温度
60 °C

実験手順

A mixture of chloromethyl ethyl carbonate (22.7 mg, 164 μmol) and NaI (24.5 mg, 164 μmol) in acetone (2.0 mL, 27 mmol) was stirred at 60° C. for 1 hour, then cooled to room temperature and added to a mixture of (R)-3-[N-(3′-chlorobiphenyl-4-ylmethyl)-N′-(3-hydroxyisoxazole-5-carbonyl)hydrazino]-2-hydroxypropionic acid 2-oxo-2-phenylethyl ester (30.0 mg, 54.5 μmol) and cesium carbonate (17.8 mg, 0.054.5 μmol) in acetone (1 mL). The resulting mixture was stirred at room temperature for 2 hours, concentrated, dissolved in AcOH (2 mL), filtered, and purified by reverse phase preparative HPLC. The desired fractions were combined and concentrated. Zinc (178 mg, 2.7 mmol) and AcOH (1.0 mL, 18 mmol) were added and the resulting mixture was stirred at room temperature for 2 hours. The mixture was filtered and purified by reverse phase preparative HPLC to yield the title compound (2.2 mg). MS m/z [M+H]+ calc'd for C24H24ClN3O9, 534.12. found 534.3.

後処理

  1. temperaturecooled to room temperature
  2. stirringThe resulting mixture was stirred at room temperature for 2 hours
  3. concentrationconcentrated
  4. dissolutiondissolved in AcOH (2 mL)
  5. filtrationfiltered
  6. custompurified by reverse phase preparative HPLC
  7. concentrationconcentrated
  8. stirringthe resulting mixture was stirred at room temperature for 2 hours
  9. filtrationThe mixture was filtered
  10. custompurified by reverse phase preparative HPLC

出典と根拠

ORDレコード
ord-b805ed5bc36f44faba74f255e66a46f6
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

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