Triethylamine → HCID 11675083, 화합물

HRID 631875노트

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HRID 631875 반응식
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]

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 10796Cesium carbonateHCID 136809Benzophenone imineHCID 11566253HCID 11566253, 화합물2회

생성물 1

HCID 11675083HCID 11675083, 화합물

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)촉매HCID 312751,4-Dioxane용매2회

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온도
100 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cd225b3c05224c1d9d141cb68ba8ffbe
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321740B2

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