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Chlorotrimethylsilane → HCID 118024047、化合物

HRID 2171783
ノート
印刷プレビュー

反応式

HRID 2171783 の反応式
BrC(Br)C.C[Si](Cl)(C)C.[C:10]([O:18][CH2:19]I)(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.Cl[C:22]1[C:23]2[N:31]=[C:30]([CH:32]3[CH2:37][CH2:36][C:35]([CH3:39])([CH3:38])[CH2:34][CH2:33]3)[S:29][C:24]=2[N:25]=[C:26]([CH3:28])[N:27]=1>C1COCC1.[Zn].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:10]([O:18][CH2:19][C:22]1[C:23]2[N:31]=[C:30]([CH:32]3[CH2:37][CH2:36][C:35]([CH3:39])([CH3:38])[CH2:34][CH2:33]3)[S:29][C:24]=2[N:25]=[C:26]([CH3:28])[N:27]=1)(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
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 4

HCID 6397ChlorotrimethylsilaneHCID 112011,1-DibromoethaneHCID 10015543Iodomethyl BenzoateHCID 118023992HCID 118023992、化合物

生成物 1

HCID 118024047HCID 118024047、化合物収率 94.7%

試薬・触媒・溶媒 3

HCID 23994Zinc触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒3 回

実験手順

Under an argon atmosphere, to a suspension of zinc powder (7.5 g) in THF (50 mL) were added dibromoethane (200 μL) and trimethylsilylchloride (200 μL), and then a solution of iodomethyl benzoate (15 g) in THF (50 mL) was added thereto, followed by stirring at room temperature for 1 hour. Then, a solution of 7-chloro-2-(4,4-dimethylcyclohexyl)-5-methyl[1,3]thiazolo[5,4-d]pyrimidine (10.9 g) in THF (50 mL) and Pd(PPh3)4 (4.25 g) were added thereto, followed by stirring at room temperature for 15 hours. The reaction mixture was filtered through Celite and then concentrated under reduced pressure. To the residue was added a 1 M aqueous NH4Cl solution, followed by extraction with EtOAc. To the organic layer were added MgSO4 and basic silica gel, followed by stirring, filtrating, and then concentrating under reduced pressure. The residue was purified by silica gel column (hexane/EtOAc) to obtain [2-(4,4-dimethylcyclohexyl)-5-methyl[1,3]thiazolo[5,4-d]pyrimidin-7-yl]methyl benzoate (13.8 g).

後処理

  1. stirringby stirring at room temperature for 15 hours
  2. filtrationThe reaction mixture was filtered through Celite
  3. concentrationconcentrated under reduced pressure
  4. additionTo the residue was added a 1 M aqueous NH4Cl solution
  5. extractionfollowed by extraction with EtOAc
  6. additionTo the organic layer were added MgSO4 and basic silica gel
  7. stirringby stirring
  8. filtrationfiltrating
  9. concentrationconcentrating under reduced pressure
  10. customThe residue was purified by silica gel column (hexane/EtOAc)

出典と根拠

ORDレコード
ord-0186f5e0c40647d0993a9eeb7f712cb9
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051339B2

反応ノート

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