Diiodomethane → HCID 15341799、化合物

HRID 1033626ノート

反応式

HRID 1033626 の反応式
[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH2:16]([Al](CC(C)C)CC(C)C)C(C)C.C(I)I.[OH-].[Na+]>C(Cl)Cl>[CH:13]1([CH2:12][C:11]2[C:2]([OH:1])=[C:3]([CH:8]=[CH:9][C:10]=2[OH:15])[C:4]([O:6][CH3:7])=[O:5])[CH2:16][CH2:14]1

参加物

6

反応物 4

HCID 6346DiiodomethaneHCID 14798Sodium HydroxideHCID 13019279Methyl 2,4-dihydroxy-3-(prop-2-en-1-yl)benzoateHCID 16682931Triisobutylaluminum

生成物 1

HCID 15341799HCID 15341799、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

The compound of Example 5 (1.0 g, 4.8 mMol) was dissolved in methylene chloride (20 cm3) and transferred to a 100 ml three-neck round bottom flask under an argon atmosphere at 0° C. Triisobutylaluminum (2.95 g, 3.76 ml, 14.9 mmol) was added dropwise via a dropping funnel. The reaction mixture was stirred for about 20 minutes while maintaining the temperature at 0° C., then methylene iodide (1.67 g, 0.5 ml, 6.2 mmol) was added via syringe, and the reaction mixture was stirred at room temperature for about four hours then slowly poured into an ice cold solution of 10% sodium hydroxide. The aqueous layer was extracted twice with about 25 ml of methylene chloride, and all of the organic fractions were combined, dried over magnesium sulfate and concentrated in vacuo to give the product.

後処理

  1. customtransferred to a 100 ml three-neck round bottom flask under an argon atmosphere at 0° C
  2. stirringthe reaction mixture was stirred at room temperature for about four hours
  3. extractionThe aqueous layer was extracted twice with about 25 ml of methylene chloride
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give the product

出典と根拠

ORDレコード
ord-572fe1be1ce447bb8613c5b23cab8d93
出典データセット
uspto-grants-1994_05
特許番号
US05310951

反応ノート

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