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

1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → 10-Oxo-dec-7-ene-1-sulfonic acid hexylamide

HRID 1779193
ノート
印刷プレビュー

反応式

HRID 1779193 の反応式
[CH2:1]([NH:7][S:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]/[CH:17]=[CH:18]/[CH2:19][C:20](O)=[O:21])(=[O:10])=[O:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C([C@H]1C(C2C=CC=CC=2)(C2C=CC=CC=2)OC(=S)N1)(C)C.Cl.C(N=C=NCCCN(C)C)C.P([O-])(O)(O)=O.[Na+]>ClCCl.CN(C1C=CN=CC=1)C.C(OCC)(=O)C>[CH2:1]([NH:7][S:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH:17]=[CH:18][CH2:19][CH:20]=[O:21])(=[O:10])=[O:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]
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 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 23672064Monosodium phosphateHCID 39058337(S)-4-Isopropyl-5,5-diphenyloxazolidine-2-thioneHCID 90060320(E)-10-hexylsulfamoyl-dec-3-enoic acid

生成物 1

HCID 13173485910-Oxo-dec-7-ene-1-sulfonic acid hexylamide収率 101.6%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

Under a nitrogen atmosphere, (E)-10-hexylsulfamoyl-dec-3-enoic acid (100 mg, 0.30 mmol) obtained in Step C-3 and (S)-4-isopropyl-5,5-diphenyl-oxazolidine-2-thione (89.2 mg, 0.30 mmol) were dissolved in dichloromethane (3.5 mL), and the mixture was cooled to 0° C. While maintaining the temperature at 0° C., N,N-dimethyl-4-aminopyridine (3.7 mg, 0.03 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (74.7 mg, 0.39 mmol) were added in order, and the mixture was stirred at 0° C. for 2 minutes and at room temperature for 13 hours. To the reaction solution was added an aqueous solution (4.2 mL) of 10% sodium dihydrogen phosphate and ethyl acetate and the mixture was extracted. The organic layer was washed with water and a saturated brine in order, dried over anhydrous sodium sulfate, and filtered. The solvent was distilled off. The resulting residue was then purified with SP1 (SiO2 cartridge, 20% ethyl acetate/n-hexane, Rf=0.25) to obtain the target compound, (E)-104(S)-4-isopropyl-5,5-diphenyl-2-thioxo-oxazolidin-3-yl)-10-oxo-dec-7-ene-1-sulfonic acid hexylamide (ESI (LC/MS positive mode) m/z 613 (M+H); Rt 2.60 min.; 65% purity, 96.8 mg, 53% yield).

後処理

  1. temperatureWhile maintaining the temperature at 0° C.
  2. extractionthe mixture was extracted
  3. washThe organic layer was washed with water
  4. dry with materiala saturated brine in order, dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. distillationThe solvent was distilled off
  7. customThe resulting residue was then purified with SP1 (SiO2 cartridge, 20% ethyl acetate/n-hexane, Rf=0.25)

出典と根拠

ORDレコード
ord-bf6995f69dd345afa9420280028f52bb
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09266853B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート