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

HRID 256854

반응식

HRID 256854 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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°.

후처리

  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°

출처 및 근거

ORD 기록
ord-c086264cb3754d7dbd62c47068519986
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05260294

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