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Propyne → ethyl 8-prop-1-ynyl-6-(trifluoromethoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylate

HRID 854908
ノート
印刷プレビュー

反応式

HRID 854908 の反応式
IC1[CH:3]=[C:4]([O:21][C:22]([F:25])([F:24])[F:23])[CH:5]=[C:6]2[C:11]=1[O:10][CH:9]([C:12]([F:15])([F:14])[F:13])[C:8]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:7]2.[CH2:26](Cl)Cl.[CH:29]#[C:30][CH3:31]>C1(C)C=CC=CC=1.[Cl-].[Na+].O.[Cu]I.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[C:30]([C:31]1[CH:3]=[C:4]([O:21][C:22]([F:25])([F:23])[F:24])[CH:5]=[C:6]2[C:11]=1[O:10][CH:9]([C:12]([F:13])([F:14])[F:15])[C:8]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:7]2)#[C:29][CH3:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 6335Propyne2 回HCID 6344Dichloromethane2 回HCID 86599457ethyl 8-iodo-6-(trifluoromethoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylate

生成物 1

HCID 86599459ethyl 8-prop-1-ynyl-6-(trifluoromethoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylate収率 89%

試薬・触媒・溶媒 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒2 回
HCID 1140Toluene溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

To a Parr bottle containing a mixture of ethyl 8-iodo-6-(trifluoromethoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylate prepared as in Example 21 a, Step 2 (0.500 g, 1.04 mmole), CuI (20 mg, 0.104 mmole), PdCl2(dppf)2.CH2Cl2 (84.5 mg, 0.104 mmole) and TEA (434 uL, 3.11 mmole) in anhydrous toluene (10 mL) was added at −78° C. propyne (2 ml) and the bottle was sealed. After stirring for 23 h at room temperature, an additional propyne (5 ml) was added and the mixture was stirred an additional 23 h at room temperature. Additional PdCl2(dppf)2.CH2Cl2 (120 mg, 0.147 mmole) was added and the mixture was stirred at room temperature for an additional 24 h. The mixture was then poured into brine (100 mL) and extracted with EtOAc (200 mL). The EtOAc layer was separated, dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by silica chromatography (9:1 hexanes:EtOAc) to give 0.363 g (89% yield) of the product as a yellow crystalline solid: EIHRMS m/z 394.0644 (M+, C17H12F6O4, Calc'd 394.0640).

後処理

  1. additionTo a Parr bottle containing
  2. customthe bottle was sealed
  3. stirringthe mixture was stirred an additional 23 h at room temperature
  4. stirringthe mixture was stirred at room temperature for an additional 24 h
  5. extractionextracted with EtOAc (200 mL)
  6. customThe EtOAc layer was separated
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by silica chromatography (9:1 hexanes:EtOAc)

出典と根拠

ORDレコード
ord-2455429601cd4ea0a35f009180254359
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07259266B2

反応ノート

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