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Potassium Carbonate → N-[6-(3-Ethoxypropoxy)-2,2-dimethylchroman-4-yl]-N-ethyl-methanesulfonamide

HRID 567060
ノート
印刷プレビュー

反応式

HRID 567060 の反応式
[CH3:1][C:2]1([CH3:20])[CH2:11][CH:10]([N:12]([CH2:17][CH3:18])[S:13]([CH3:16])(=[O:15])=[O:14])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([OH:19])[CH:8]=2)[O:3]1.C(=O)([O-])[O-].[K+].[K+].[CH2:27]([O:29][CH2:30][CH2:31][CH2:32]Br)[CH3:28]>CC(N(C)C)=O>[CH2:27]([O:29][CH2:30][CH2:31][CH2:32][O:19][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[O:3][C:2]([CH3:1])([CH3:20])[CH2:11][CH:10]2[N:12]([CH2:17][CH3:18])[S:13]([CH3:16])(=[O:15])=[O:14])[CH3:28]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2604931-bromo-3-ethoxypropaneHCID 17786837N-[2,2-dimethyl-6-hydroxychroman-4-yl]-N-ethyl-methanesulfonamide

生成物 1

HCID 9886441N-[6-(3-Ethoxypropoxy)-2,2-dimethylchroman-4-yl]-N-ethyl-methanesulfonamide

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
110 °C

実験手順

1.5 g (5 mmol) of N-[2,2-dimethyl-6-hydroxychroman-4-yl]-N-ethyl-methanesulfonamide were heated to 80° C. for 30 min with 1.38 g (10 mmol) of powdered potassium carbonate in 60 ml of DMA. 4 ml of 3-ethoxy-1-bromopropane were then added dropwise at 50-60° C., the mixture was heated to 110° C. for 2 h and concentrated in vac. after cooling, the residue was treated with water and aqueous hydrochloric acid, the mixture was extracted with EA, the organic phase was dried and concentrated, and the oily residue was chromatographed on silica gel using n-heptane/EA (2:1). 0.9 g of N-[6-(3-ethoxypropoxy)-2,2-dimethylchroman-4-yl]-N-ethyl-methanesulfonamide was crystallized from appropriate fractions using petroleum ether, m.p. 72-74° C.

後処理

  1. concentrationconcentrated in vac
  2. temperatureafter cooling
  3. additionthe residue was treated with water and aqueous hydrochloric acid
  4. extractionthe mixture was extracted with EA
  5. customthe organic phase was dried
  6. concentrationconcentrated
  7. customthe oily residue was chromatographed on silica gel
  8. custom0.9 g of N-[6-(3-ethoxypropoxy)-2,2-dimethylchroman-4-yl]-N-ethyl-methanesulfonamide was crystallized from appropriate fractions

出典と根拠

ORDレコード
ord-03afe92e828542c797867983fd3439bf
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06177449B1

反応ノート

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