Water → HCID 59637737、化合物

HRID 1892019ノート

反応式

HRID 1892019 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([O:9][CH2:10][C:11]#[C:12][Si:13]([CH3:16])([CH3:15])[CH3:14])=[O:8].[K].[C:18]1(=[O:28])[NH:22][C:21](=[O:23])[C:20]2=[CH:24][CH:25]=[CH:26][CH:27]=[C:19]12.C(Cl)(Cl)Cl.O>CN(C=O)C>[C:18]1(=[O:28])[N:22]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([O:9][CH2:10][C:11]#[C:12][Si:13]([CH3:16])([CH3:15])[CH3:14])=[O:8])[C:21](=[O:23])[C:20]2=[CH:24][CH:25]=[CH:26][CH:27]=[C:19]12

参加物

6

反応物 4

HCID 962WaterHCID 6212ChloroformHCID 24194345Phthalimide potassium saltHCID 59637735HCID 59637735、化合物

生成物 1

HCID 59637737HCID 59637737、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-(trimethylsilyl)prop-2-ynyl 6-bromohexanoate (0.606 g, 2 mmol, 1 eq.) was added to a solution of phthalimide potassium salt (0.4412 g, 2.4 mmol, 1.2 eq.) in 50 mL of DMF and stirred overnight under argon. CHCl3 was added to the solution flask and was transferred to a separatory funnel containing water. The aqueous layer was separated and twice extracted with CHCl3. The combined organic layers were twice extracted with water then the solvent was removed on a rotary evaporator. Remaining solvent was removed under high vacuum overnight to yield a brown oil.

後処理

  1. customwas transferred to a separatory funnel
  2. customThe aqueous layer was separated
  3. extractiontwice extracted with CHCl3
  4. extractionThe combined organic layers were twice extracted with water
  5. customthe solvent was removed on a rotary evaporator
  6. customRemaining solvent was removed under high vacuum overnight
  7. customto yield a brown oil

出典と根拠

ORDレコード
ord-1ca5145ce0074dfaa3e8a06dbd24ecd4
出典データセット
uspto-grants-2013_08
特許番号
US08507572B2

反応ノート

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