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1,2-Dibromoethane → HCID 66922349、化合物

HRID 2039837
ノート
印刷プレビュー

反応式

HRID 2039837 の反応式
BrCCBr.[F:5][C:6]1[C:7]([CH3:14])=[C:8]([CH:11]=[CH:12][CH:13]=1)[CH2:9]Br.[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][N:25]([C:28]([C:30]2[C:34]3[CH:35]=[N:36][C:37]([O:39][CH3:40])=[CH:38][C:33]=3[N:32]([C:41]3[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=3)[C:31]=2Cl)=[O:29])[CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:17])[CH3:16].COC1C=CC=C(OC)C=1C1C=CC=CC=1P(C1CCCCC1)C1CCCCC1>C1COCC1.CCCCCC.[Zn].C([O-])(=O)C.[Pd+2].C([O-])(=O)C.Cl[Si](C)(C)C.CN(C=O)C>[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][N:25]([C:28]([C:30]2[C:34]3[CH:35]=[N:36][C:37]([O:39][CH3:40])=[CH:38][C:33]=3[N:32]([C:41]3[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=3)[C:31]=2[CH2:9][C:8]2[CH:11]=[CH:12][CH:13]=[C:6]([F:5])[C:7]=2[CH3:14])=[O:29])[CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:16])[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 4

HCID 78391,2-DibromoethaneHCID 27792443-Fluoro-2-methylbenzyl bromideHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 66922140HCID 66922140、化合物

生成物 1

HCID 66922349HCID 66922349、化合物収率 76%

試薬・触媒・溶媒 6

HCID 6397
Chlorotrimethylsilane
触媒
HCID 23994Zinc触媒
HCID 167845palladium(II) acetate触媒
HCID 6228Dimethylformamide溶媒
HCID 8028Tetrahydrofuran溶媒2 回
HCID 8058Hexane溶媒

実験手順

To zinc (167 mg, 2.55 mmol) in dry THF (500 μl) in a dry flask under an argon atmosphere was added 1,2-dibromoethane (5.49 μl, 63.7 μmol). The mixture was heated three times to reflux with a heat gun and allowed to cool to room temperature. Then chlorotrimethylsilane (0.27 μl, 2.12 μmol) was added and the mixture was stirred at room temperature for 20 min. Subsequently the flask was placed in an ice bath and a solution of 3-fluoro-2-methyl-benzylbromide (259 mg, 1.27 mmol) in dry THF (1 ml) was added slowly so that the temperature remained at 0° C. The mixture was stirred at 0° C. for 4.5 h and placed in the refrigerator overnight. Then the cooled mixture was added dropwise to a precooled solution (−78° C.) of B-OM-9-BBN (2.12 ml, 2.12 mmol, 1 M) in hexane. The mixture was stirred at room temperature for 30 min. DMF (5 ml) was added, followed by the compound of step 6 (100 mg, 212 μmol), palladium(II) acetate (4.77 mg, 21.2 μmol) and S—PHOS (17.4 mg, 42.5 μmol). The reaction mixture was stirred at 100° C. for 3 h. After cooling, the mixture was quenched with water and extracted with EA. The organic layer was dried over sodium sulfate, filtered, and evaporated under reduced pressure. The residue was purified by silica gel chromatography (EA (10 to 60%) HEP) to give 90 mg of the title compound.

後処理

  1. temperatureThe mixture was heated three times
  2. temperatureto reflux with a heat gun
  3. customSubsequently the flask was placed in an ice bath
  4. customremained at 0° C
  5. stirringThe mixture was stirred at 0° C. for 4.5 h
  6. customplaced in the refrigerator overnight
  7. stirringThe mixture was stirred at room temperature for 30 min
  8. stirringThe reaction mixture was stirred at 100° C. for 3 h
  9. temperatureAfter cooling
  10. customthe mixture was quenched with water
  11. extractionextracted with EA
  12. dry with materialThe organic layer was dried over sodium sulfate
  13. filtrationfiltered
  14. customevaporated under reduced pressure
  15. customThe residue was purified by silica gel chromatography (EA (10 to 60%) HEP)

出典と根拠

ORDレコード
ord-7e8688ad9c5a45f1ad2a21b30b725962
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08580813B2

反応ノート

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