Triethylamine → HCID 11675083、化合物

HRID 631875ノート

反応式

HRID 631875 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].C(N(CC)CC)C.[CH3:14][O:15][C:16]([C:18]1[C:27]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]=2[CH:21]=[CH:20][C:19]=1OS(C(F)(F)F)(=O)=O)=[O:17].[C:36](=[NH:49])([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>[CH3:14][O:15][C:16]([C:18]1[C:27]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]=2[CH:21]=[CH:20][C:19]=1[N:49]=[C:36]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)=[O:17]

参加物

8

反応物 4

HCID 8471TriethylamineHCID 10796Cesium carbonateHCID 136809Benzophenone imineHCID 11566253HCID 11566253、化合物2 回

生成物 1

HCID 11675083HCID 11675083、化合物

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)触媒HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
100 °C

実験手順

Cesium carbonate (12.4 g), palladium (II) acetate (0.12 g), triethylamine (0.12 mL) and Xantphos (0.474 g) were suspended in dioxane (50 mL) under nitrogen. 2-Trifluoromethanesulfonyloxy-5,6,7,8-tetrahydronaphthalene-1-carboxylic acid methyl ester (Intermediate 7, 4.2 g) and benzhydrylidenamine (5.5 mL) in dioxane (35 mL) were added and the mixture was heated at 100° C. for 3.5 hours. The resulting mixture was partitioned between ethyl acetate and water. The organic solution was washed with water and concentrated under vacuum. The residue was recrystallised from methanol to give the title compound as an off-white solid (8.2 g).

後処理

  1. customThe resulting mixture was partitioned between ethyl acetate and water
  2. washThe organic solution was washed with water
  3. concentrationconcentrated under vacuum
  4. customThe residue was recrystallised from methanol

出典と根拠

ORDレコード
ord-cd225b3c05224c1d9d141cb68ba8ffbe
出典データセット
uspto-grants-2016_04
特許番号
US09321740B2

反応ノート

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