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Tetrahydrofuran → 2-Cyclohexylmethyl-benzothiazole-6-carbonitrile

HRID 911573
ノート
印刷プレビュー

反応式

HRID 911573 の反応式
Br[C:2]1[S:3][C:4]2[CH:10]=[C:9]([C:11]#[N:12])[CH:8]=[CH:7][C:5]=2[N:6]=1.C1COCC1.[Br-].[CH:19]1([CH2:25][Zn+])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].CN1CCCC1=O>[CH:19]1([CH2:25][C:2]2[S:3][C:4]3[CH:10]=[C:9]([C:11]#[N:12])[CH:8]=[CH:7][C:5]=3[N:6]=2)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]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

7

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 252588342-Bromobenzo[d]thiazole-6-carbonitrileHCID 178419774HCID 178419774、化合物

生成物 1

HCID 667067722-Cyclohexylmethyl-benzothiazole-6-carbonitrile収率 57%

試薬・触媒・溶媒 3

HCID 67553Tetrabutylammonium Iodide触媒
HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
80 °C

実験手順

Place 2-bromo-benzothiazole-6-carbonitrile (0.2 g, 0.96 mmol), anhydrous THF (3 mL), 1-methyl-2-pyrrolidinone (3 mL), tetrabutylammonium iodide (1.1 g, 2.89 mmol), tris(dibenzylideneacetone)dipalladium(0) (18 mg, 0.09 mmol) and [1,1′-bis(diphenylphosphino)ferrocine]dichloropalladium (II) (11 mg, 0.09 mmol) in a flask. Add 0.5M cyclohexylmethylzinc bromide in THF (3.8 mL, 1.92 mmol) to the mixture, degas 3 times by partially evacuating the atmosphere and flushing with nitrogen and stir the reaction mixture at 80° C. for 2 h. Cool the reaction mixture to room temperature, dilute with EtOAc (10 mL) and wash with brine (10 mL). Dry the organic layer over anhydrous Na2SO4, filter and concentrate in vacuo. Purity the residue by chromatography on silica gel eluting sequentially with hexane/EtOAc (1:0 to 4:1 gradient) to obtain the desired intermediate as a yellow solid (140 mg, 57%). GC-MS m/z: 256 (M+).

後処理

  1. customdegas 3 times
  2. customby partially evacuating the atmosphere
  3. customflushing with nitrogen
  4. temperatureCool the reaction mixture to room temperature
  5. additiondilute with EtOAc (10 mL)
  6. washwash with brine (10 mL)
  7. dry with materialDry the organic layer over anhydrous Na2SO4
  8. filtrationfilter
  9. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-a3e65b8c4beb4fda9756db4a3b5ff877
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08022062B2

反応ノート

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