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Tetrahydrofuran → HCID 178421673、化合物

HRID 2112525
ノート
印刷プレビュー

反応式

HRID 2112525 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([CH3:20])[C:17]([CH3:19])=[CH:18][C:13]=2[N:12]=[C:11]2[N:21](CC=C)[NH:22][C:23]([CH3:24])=[C:10]2[N:9]=1.O1CCCC1.[H-].C([Al+]CC(C)C)C(C)C>C1(C)C=CC=CC=1.[Ni](Cl)Cl.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([CH3:20])[C:17]([CH3:19])=[CH:18][C:13]=2[N:12]=[C:11]2[NH:21][NH:22][C:23]([CH3:24])=[C:10]2[N:9]=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

6

反応物 3

HCID 8028TetrahydrofuranHCID 21225700DiisobutylaluminumhydrideHCID 178456639HCID 178456639、化合物

生成物 1

HCID 178421673HCID 178421673、化合物収率 62.2%

試薬・触媒・溶媒 2

HCID 2724937Dichloro(1,1'-(1,3-propanediyl)bis(1,1-diphenylphosphine-kappaP))nickel触媒
HCID 1140
Toluene
溶媒

反応条件

温度
0 °C

実験手順

To a solution of 2.7 g (0.00716 mole) of 5-(2-chlorophenyl)-1,2-dihydro-3,7,8-trimethyl-1-(2-propenyl)-pyrazolo[3,4-b][1,4]benzodiazepine (XIVw), 0.155 g (0.00029 mole) of 1,3-bis(diphenylphosphino)propane nickel (II) chloride and 140 mL of anhydrous tetrahydrofuran at −40° C. was added 43 mL of 1M diisobutylaluminum hydride in toluene. The mixture was stirred at 0° C. for 6 hours and then quenched by the careful addition of ice water. The mixture was extracted twice with ethyl acetate. The combined ethyl acetate extracts were dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with ethyl acetate-dichloromethane (1:1) to give 1.5 g of 5-(2-chlorophenyl)-1,2-dihydro-3,7,8-trimethyl-pyrazolo[3,4-b][1,4]benzodiazepine (IVw) as an orange solid. MH+/Z=337.

後処理

  1. customquenched by the careful addition of ice water
  2. extractionThe mixture was extracted twice with ethyl acetate
  3. dry with materialThe combined ethyl acetate extracts were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography
  7. washeluting with ethyl acetate-dichloromethane (1:1)

出典と根拠

ORDレコード
ord-f9c8b93143ed4a3fb30525e2f2e8244b
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07524840B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート