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Hydrochloric Acid → 3,4-Dihydro-2-(2-dimethylaminoethyl)-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol

HRID 846172
ノート
印刷プレビュー

反応式

HRID 846172 の反応式
Br[CH2:2][CH2:3][C:4]1([CH3:18])[CH2:9][CH2:8][C:7]2[C:10]([CH3:17])=[C:11]([OH:16])[C:12]([CH3:15])=[C:13]([CH3:14])[C:6]=2[O:5]1.[CH3:19][NH:20][CH3:21].O.[ClH:23]>CN(C)C=O.C(O)(C)C>[ClH:23].[CH3:19][N:20]([CH3:21])[CH2:2][CH2:3][C:4]1([CH3:18])[CH2:9][CH2:8][C:7]2[C:10]([CH3:17])=[C:11]([OH:16])[C:12]([CH3:15])=[C:13]([CH3:14])[C:6]=2[O:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 962WaterHCID 133751842-(2-Bromoethyl)-2,5,7,8-tetramethylchroman-6-ol

生成物 1

HCID 1312423,4-Dihydro-2-(2-dimethylaminoethyl)-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of 12.53 g of 3,4-dihydro-2-(2-bromoethyl)-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol and liquid dimethylamine in 50 ml of dimethylformamide is stirred at room temperature for 16 hours. Water is added and the product is extracted with ethyl ether. The extract is washed with water, dried over anhydrous sodium sulfate, filtered and evaporated. One equivalent of hydrochloride acid in isopropanol is added and the resulting precipitate is recrystallized twice from isopropanol/water to yield 9.44 g of the title compound, m.p. >300° C.

後処理

  1. extractionthe product is extracted with ethyl ether
  2. washThe extract is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customthe resulting precipitate is recrystallized twice from isopropanol/water

出典と根拠

ORDレコード
ord-9d9c824fae49456d981ae5dd8a7a42ad
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05135945

反応ノート

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