Dichloromethane → HCID 86605947、化合物

HRID 2252531ノート

反応式

HRID 2252531 の反応式
[CH2:1]([C:5]([CH2:10][CH:11]([CH3:13])[CH3:12])([CH2:8][OH:9])[CH2:6][OH:7])[CH:2]([CH3:4])[CH3:3].ClCCl.[CH3:17][Si:18](Cl)([CH3:20])[CH3:19]>C(N(CC)CC)C>[CH2:1]([C:5]([CH2:10][CH:11]([CH3:13])[CH3:12])([CH2:6][O:7][Si:18]([CH3:20])([CH3:19])[CH3:17])[CH2:8][O:9][Si:18]([CH3:20])([CH3:19])[CH3:17])[CH:2]([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 6397ChlorotrimethylsilaneHCID 39856252,2-Diisobutyl-1,3-propanediol

生成物 1

HCID 86605947HCID 86605947、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

0.9 g of 2,2-diisobutyl-1,3-propandiol was admixed with 20 ml of dichloromethane. The mixture was cooled in ice-water bath, thereto was added 2.0 ml of triethyl amine, followed by the addition of 1.58 ml of trimethylsilyl chloride. The mixture was stirred in ice-water bath for further 2 hours. The reaction mixture was washed with water, and the organic layer separated was dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated to give 1.45 g of concentrate. The crude product was purified by column chromatography using petroleum ether as eluent, to give colorless pure compound.

後処理

  1. washThe reaction mixture was washed with water
  2. customthe organic layer separated
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. filtrationAfter filtration
  5. customthe filtrate was evaporated
  6. customto give 1.45 g
  7. concentrationof concentrate
  8. customThe crude product was purified by column chromatography
  9. customto give colorless pure compound

出典と根拠

ORDレコード
ord-44eb9c38d5e94be1a82e89b5af99cf6c
出典データセット
uspto-grants-2008_01
特許番号
US07323431B2

反応ノート

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