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Dimethylformamide → 4-((3-aminophenyl)ethynyl)-1H-indazol-3-amine

HRID 589914
ノート
印刷プレビュー

反応式

HRID 589914 の反応式
CN(C=O)C.I[C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[C:9]([NH2:16])=[N:10][NH:11]2.[C:17]([C:19]1[CH:20]=[C:21]([CH:23]=[CH:24][CH:25]=1)[NH2:22])#[CH:18].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cu](I)I.C(N(CC)CC)C>[NH2:22][C:21]1[CH:20]=[C:19]([C:17]#[C:18][C:7]2[CH:15]=[CH:14][CH:13]=[C:12]3[C:8]=2[C:9]([NH2:16])=[N:10][NH:11]3)[CH:25]=[CH:24][CH:23]=1
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 6228DimethylformamideHCID 11776TriphenylphosphineHCID 104682Benzenamine, 3-ethynyl-HCID 40577874-iodo-1H-indazol-3-amine

生成物 1

HCID 1186384254-((3-aminophenyl)ethynyl)-1H-indazol-3-amine

試薬・触媒・溶媒 3

HCID 83717Copper iodide触媒
HCID 6102075
Dichlorobis(triphenylphosphine)palladium
触媒
HCID 8471Triethylamine溶媒

反応条件

温度
60 °C

実験手順

To 8 ml of DMF was added 4-iodo-1H-indazol-3-amine (690 mg, 2.65 mmol) and 3-ethynylaniline (480 mg, 1.5 eq., 4.1 mmol). Following that, Bis(triphenylphosphine) palladium(II) dichloride (180 mg, 0.25 mmol, 10 mol %), Copper Iodide (100 mg, 0.52 mmol, 20 mol %), Triphenylphosphine (18 mg, 0.07 mmol, 3 mol %) and 8 ml of triethylamine was added. Nitrogen was bubbled through the reaction mixture for 15 minutes. The reaction was then set with a reflux condenser, set under nitrogen atmosphere, and heated at 60° C. for 2 hours. After that, the reaction was cooled to room temperature and 40 ml of ethyl acetate was added. The organic layer was extracted with aqueous sodium bicarbonate (3×40 ml), brine (3×40 ml), dried using anhydrous sodium sulfate, loaded onto silica and columned to give 4-((3-aminophenyl)ethynyl)-1H-indazol-3-amine.

後処理

  1. additionwas added
  2. customNitrogen was bubbled through the reaction mixture for 15 minutes
  3. customThe reaction was then set with a reflux condenser
  4. temperatureAfter that, the reaction was cooled to room temperature
  5. addition40 ml of ethyl acetate was added
  6. extractionThe organic layer was extracted with aqueous sodium bicarbonate (3×40 ml), brine (3×40 ml)
  7. customdried

出典と根拠

ORDレコード
ord-e1fda866a7f34f3db769165eb6f574ac
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09233968B1

反応ノート

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