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

Triethylamine → 3-Dipropylamino-5-methyloxycarbonylchroman

HRID 2257305
ノート
印刷プレビュー

反応式

HRID 2257305 の反応式
[CH2:1]([N:4]([CH2:22][CH2:23][CH3:24])[CH:5]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][C:12]=2S(C(F)(F)F)(=O)=O)[O:7][CH2:6]1)[CH2:2][CH3:3].C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C.CN(C)[CH:63]=[O:64].[CH3:66][OH:67]>C1(C)C=CC=CC=1>[CH2:1]([N:4]([CH2:22][CH2:23][CH3:24])[CH:5]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][C:12]=2[C:66]([O:64][CH3:63])=[O:67])[O:7][CH2:6]1)[CH2:2][CH3:3]
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

6

反応物 4

HCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 190281063-Dipropylamino-5-trifluoromethanesulfonylchromanHCID 21901440N,N-dimethylformamide methanol

生成物 1

HCID 190280933-Dipropylamino-5-methyloxycarbonylchroman

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

反応条件

温度
70 °C

実験手順

3-Dipropylamino-5-trifluoromethanesulfonylchroman (Example 1; 4.43 g, 11.6 mmol) was dissolved in 80 mL dimethylformamide/methanol 6:2 and the solution was degassed (10 mm Hg, 20° C., 15 min). PdOAc2 (76 mg, 0.34 mmol), 1,3-bis-diphenylphosphinopropane (141 mg, 0.34 mmol) and triethylamine (3.5 mL, 25 mmol) were then added. The mixture was heated to 70° C. under CO atmosphere and stirred for 5 hours. The solution was cooled, diluted with toluene (200 mL), washed with aqueous NaHCO3, dried with Na2SO4 and evaporated to dryness. The oil was purified by flash chromatography (silica gel) by elution with ethyl acetate/hexane 1:8.

後処理

  1. customthe solution was degassed (10 mm Hg, 20° C., 15 min)
  2. temperatureThe solution was cooled
  3. washwashed with aqueous NaHCO3
  4. dry with materialdried with Na2SO4
  5. customevaporated to dryness
  6. customThe oil was purified by flash chromatography (silica gel) by elution with ethyl acetate/hexane 1:8

出典と根拠

ORDレコード
ord-0a622239fd9c4e6db79148804fee2d8a
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05656657

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