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Water → HCID 69416361、化合物

HRID 1270162
ノート
印刷プレビュー

反応式

HRID 1270162 の反応式
Br[C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([NH:17][CH:18]([CH3:20])[CH3:19])[C:8]3[N:9]2[C:12]([O:15]C)=[N:13][N:14]=3)=[CH:4][CH:3]=1.[C:21]1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C.[CH3:57][OH:58].CS(C)=O.[OH2:63]>C(Cl)Cl>[CH3:57][O:58][C:21]([C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([NH:17][CH:18]([CH3:20])[CH3:19])[C:8]3[N:9]2[C:12](=[O:15])[NH:13][N:14]=3)=[CH:4][CH:3]=1)=[O:63]
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

7

反応物 5

HCID 962WaterHCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 18449223HCID 18449223、化合物HCID 22036561Dimethyl sulfoxide methanol

生成物 1

HCID 69416361HCID 69416361、化合物

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

反応条件

温度
75 °C

実験手順

A solution of 2.0 g of (8-bromo-1-methoxy-[1,2,4]triazolo[4,3-a]quinoxalin-4-yl)-isopropyl-amine, 0.54 g of Pd(II)acetate, 0.66 g of 1,3-bis-(diphenylphosphino)propane, and triethylamine (21 mL) in a 1.1/1.0 mixture of MeOH/DMSO was agitated under an atmosphere of CO (45 psi) at 75° C. for 96 hrs. After cooling to 23° C., the solution was diluted with water and methylene chloride and the resulting mixture filtered through diatomaceous earth. The filtrate was concentrated and the residue was dissolved in methylene chloride and washed with brine (2×). The title compound precipitated from the organic layer upon standing and was isolated by filtration. MS (M+H)+=302.3.

後処理

  1. temperatureAfter cooling to 23° C.
  2. filtrationthe resulting mixture filtered through diatomaceous earth
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in methylene chloride
  5. washwashed with brine (2×)
  6. customThe title compound precipitated from the organic layer
  7. customwas isolated by filtration

出典と根拠

ORDレコード
ord-cd5b2c331dfc436d81f548adeab09221
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07202245B2

反応ノート

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