Diiodomethane → HCID 15341799, 화합물

HRID 1033626노트

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HRID 1033626 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 15341799HCID 15341799, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-572fe1be1ce447bb8613c5b23cab8d93
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310951

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