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Ammonia → HCID 16752727、化合物

HRID 2194995
ノート
印刷プレビュー

反応式

HRID 2194995 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5](I)=[CH:4][C:3]=1[C:9]1[N:18]=[CH:17][C:16]2[CH2:15][CH2:14][C:13]3[N:19]=[C:20]([NH:22][C:23](=[O:25])[CH3:24])[S:21][C:12]=3[C:11]=2[N:10]=1.[CH3:26][NH:27][CH2:28][C:29]#[CH:30].C(N(C(C)C)CC)(C)C.O=O.N>O1CCCC1.[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cu]I.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:30]#[C:29][CH2:28][NH:27][CH3:26])=[CH:4][C:3]=1[C:9]1[N:18]=[CH:17][C:16]2[CH2:15][CH2:14][C:13]3[N:19]=[C:20]([NH:22][C:23](=[O:25])[CH3:24])[S:21][C:12]=3[C:11]=2[N:10]=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

10

反応物 5

HCID 222AmmoniaHCID 977OxygenHCID 81531DiisopropylethylamineHCID 96160N-methylpropyn-2-ylamineHCID 59254920HCID 59254920、化合物

生成物 1

HCID 16752727HCID 16752727、化合物

試薬・触媒・溶媒 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 13169693Triphenylphosphine palladium dichloride触媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

1.0 g (2.1 mmol) N-[8-(2-chloro-5-iod-phenyl)-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-yl]-acetamide are placed in 50 mL tetrahydrofuran under an argon atmosphere and combined with 0.6 ml (9 mmol) N-methylpropargylamine and 1 mL (6 mmol) diisopropylethylamine. The mixture is kept free from oxygen and 29 mg (0.04 mmol) triphenylphosphine palladium(II)-chloride and 8 mg (0.04 mmol) copper(I)-iodide are added. The mixture is stirred for 5 hours at 80° C. After cooling to ambient temperature the reaction mixture is combined with water and 10% ammonia solution and extracted with dichloromethane. The organic phase is dried and evaporated to dryness. The residue is purified by chromatography, the product obtained is triturated with diethyl ether and suction filtered.

後処理

  1. additionare added
  2. temperatureAfter cooling to ambient temperature the reaction mixture
  3. extractionextracted with dichloromethane
  4. customThe organic phase is dried
  5. customevaporated to dryness
  6. customThe residue is purified by chromatography
  7. customthe product obtained
  8. customis triturated with diethyl ether and suction
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-9a5684583c124713b8f3efa1dcca2a5f
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08334378B2

反応ノート

読み込み中…

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