Hexane → [1-(6-Benzyloxy-2-naphthylmethyl)-4-phenyl-3-pyrrolyl]methanol

HRID 349894

반응식

HRID 349894 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:14][C:15]1[CH:16]=[C:17]2[C:22](=[CH:23][CH:24]=1)[CH:21]=[C:20]([CH2:25][N:26]1[CH:30]=[C:29]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[C:28]([C:37](OC)=[O:38])=[CH:27]1)[CH:19]=[CH:18]2)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].CCCCCC>O1CCCC1>[CH2:7]([O:14][C:15]1[CH:16]=[C:17]2[C:22](=[CH:23][CH:24]=1)[CH:21]=[C:20]([CH2:25][N:26]1[CH:30]=[C:29]([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)[C:28]([CH2:37][OH:38])=[CH:27]1)[CH:19]=[CH:18]2)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

6

반응물 4

HCID 8058HexaneHCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23024964Methyl 1-(6-benzyloxy-2-naphthylmethyl)-4-phenylpyrrole-3-carboxylate

생성물 1

HCID 23024834[1-(6-Benzyloxy-2-naphthylmethyl)-4-phenyl-3-pyrrolyl]methanol수율 89.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium aluminium hydride (0.258 g) was added to a solution of methyl 1-(6-benzyloxy-2-naphthylmethyl)-4-phenylpyrrole-3-carboxylate (3.04 g) in tetrahydrofuran (30 ml) at 0° C., and the mixture was stirred at room temperature for one hour. Sodium sulfate decahydrate (2.19 g) and hexane (30 ml) were added to the reaction mixture and the mixture was stirred at room temperature for 30 minutes. After the precipitate was removed by filtration, the filtrate was concentrated. The colorless crystals obtained were collected by filtration to yield [1-(6-benzyloxy-2-naphthylmethyl)-4-phenyl-3-pyrrolyl]methanol (2.54 g, yield: 89%). This was recrystallized from ethyl acetate-hexane. Melting point: 116–117° C.

후처리

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. customAfter the precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. customThe colorless crystals obtained
  5. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-893a5b8d331c4781ae8adea75059963c
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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