Water → HCID 19068237, 화합물

HRID 1957701노트

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HRID 1957701 반응식
[H-].[Na+].[C:3]12([C:13]3[CH:14]=[C:15]([OH:21])[CH:16]=[CH:17][C:18]=3[O:19][CH3:20])[CH2:12][CH:7]3[CH2:8][CH:9]([CH2:11][CH:5]([CH2:6]3)[CH2:4]1)[CH2:10]2.Br[CH2:23][C:24]1[S:25][CH:26]=[C:27]([C:29]([O:31][CH3:32])=[O:30])[CH:28]=1.O>CN(C=O)C>[C:3]12([C:13]3[CH:14]=[C:15]([CH:16]=[CH:17][C:18]=3[O:19][CH3:20])[O:21][CH2:23][C:24]3[S:25][CH:26]=[C:27]([C:29]([O:31][CH3:32])=[O:30])[CH:28]=3)[CH2:4][CH:5]3[CH2:11][CH:9]([CH2:8][CH:7]([CH2:6]3)[CH2:12]1)[CH2:10]2

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 19068273HCID 19068273, 화합물HCID 19068282HCID 19068282, 화합물

생성물 1

HCID 19068237HCID 19068237, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

210 mg (7 mmol) of sodium hydride (80% in oil) and 10 ml of DMF were introduced into a three-necked flask under a stream of nitrogen. A solution of 1.8 g (7 mmol) of 3-(1-adamantyl)-4-methoxyphenol in 20 ml of DMF was added dropwise and the mixture was stirred until the evolution of gas had ceased. A solution of 1.7 g (7.2 mmol) of methyl 2-bromomethyl-4-thiophenecarboxylate in 15 ml of DMF was then added and the mixture was stirred at room temperature for two hours. The reaction medium was poured into water and extracted with ethyl ether. The organic phase was separated out after settling had taken place, dried over magnesium sulfate and evaporated. The solid obtained was triturated from hexane, filtered off and dried. 2.6 g (90%) of the expected methyl ester, having a melting point of 97°-8° C., were recovered.

후처리

  1. stirringthe mixture was stirred at room temperature for two hours
  2. extractionextracted with ethyl ether
  3. customThe organic phase was separated out
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customThe solid obtained
  7. customwas triturated from hexane
  8. filtrationfiltered off
  9. customdried
  10. customwere recovered

출처 및 근거

ORD 기록
ord-48c9ba880ddb4c1b8c089c75a9c73153
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786379

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