1-Iodonaphthalene → rac-3,4-dihydro-2,5,7,8-tetramethyl-2-[(1-naphthyl)ethynyl]-2H-1-benzopyran-6-ol

HRID 256854

反応式

HRID 256854 の反応式
[C:1]([C:3]1([CH3:17])[CH2:8][CH2:7][C:6]2[C:9]([CH3:16])=[C:10]([OH:15])[C:11]([CH3:14])=[C:12]([CH3:13])[C:5]=2[O:4]1)#[CH:2].I[C:19]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:22]=[CH:21][CH:20]=1>C(Cl)Cl>[CH3:17][C:3]1([C:1]#[C:2][C:27]2[C:28]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:24]=[CH:25][CH:26]=2)[CH2:8][CH2:7][C:6]2[C:9]([CH3:16])=[C:10]([OH:15])[C:11]([CH3:14])=[C:12]([CH3:13])[C:5]=2[O:4]1

参加物

4

反応物 2

HCID 70041-IodonaphthaleneHCID 14478563rac-3,4-dihydro-2-ethynyl-2,5,7,8-tetramethyl-2H-1-benzopyran-6ol

生成物 1

HCID 15171855rac-3,4-dihydro-2,5,7,8-tetramethyl-2-[(1-naphthyl)ethynyl]-2H-1-benzopyran-6-ol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

rac-3,4-dihydro-2,5,7,8-tetramethyl-2-[(1-naphthyl)ethynyl]-2H-1-benzopyran-6-ol was prepared by coupling rac-3,4-dihydro-2-ethynyl-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol with 1-iodonaphthalene under the conditions described in Example 1. It was isolated by chromatography over 40 fold amount of silica gel using methylene chloride. The combined clean fractions were crystallized from hexane and recrystallized from petroleum ether to give colorless crystals with m.p. 127°-128°.

後処理

  1. customIt was isolated by chromatography over 40 fold amount of silica gel
  2. customThe combined clean fractions were crystallized from hexane
  3. customrecrystallized from petroleum ether
  4. customto give colorless crystals with m.p. 127°-128°

出典と根拠

ORDレコード
ord-c086264cb3754d7dbd62c47068519986
出典データセット
uspto-grants-1993_11
特許番号
US05260294

関連ノート

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