Chlorotrimethylsilane → [4-Bromo-(2-indanyl)-oxy]-trimethyl silane

HRID 1646598ノート

反応式

HRID 1646598 の反応式
C(N(CC)CC)C.[Br:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH2:11][CH:12]([OH:18])[CH2:13]2.[CH3:19][Si:20](Cl)([CH3:22])[CH3:21].C(OC(C)C)(C)C>C(Cl)Cl.O>[Br:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH2:11][CH:12]([O:18][Si:20]([CH3:22])([CH3:21])[CH3:19])[CH2:13]2

参加物

7

反応物 4

HCID 6397ChlorotrimethylsilaneHCID 7914Diisopropyl EtherHCID 8471TriethylamineHCID 145152994-bromo-2,3-dihydro-1H-inden-2-ol

生成物 1

HCID 19801163[4-Bromo-(2-indanyl)-oxy]-trimethyl silane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

5.2 ml of anhydrous triethylamine is added drop by drop to 5.3 g of product obtained in Stage B in 50 ml of methylene chloride. After cooling to 0°, +5° C., 3.5 ml of trimethylsilyl chloride in 15 ml of methylene chloride is introduced drop by drop, with agitation for 5 minutes at 0° C. and for 15 minutes at ambient temperature. The reaction mixture is poured into 200 ml of a water and ice mixture and 100 ml of isopropyl ether. After decanting, the organic phase is washed with water to obtain a pH of 7.5-8, and the aqueous phases with water are extracted by isopropyl ether. The organic phases are reunited, dried, concentrated to dryness and 6.81 g of expected product is obtained.

後処理

  1. temperatureAfter cooling to 0°, +5° C.
  2. waitfor 15 minutes at ambient temperature
  3. customAfter decanting
  4. washthe organic phase is washed with water
  5. customto obtain a pH of 7.5-8
  6. extractionthe aqueous phases with water are extracted by isopropyl ether
  7. customdried
  8. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-8e6d4257a2e94499baede7feb4b2ce81
出典データセット
uspto-grants-1993_01
特許番号
US05180741

反応ノート

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