Ethanol → HCID 71089357, 화합물

HRID 1055282노트

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HRID 1055282 반응식
[CH2:1]([C:7]1([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[C:19]2[CH:18]=[C:17]3[C:20](=[O:24])[CH:21]([CH3:23])[CH2:22][C:16]3=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C(O)C.[BH4-].[Na+]>C1COCC1>[CH2:25]([C:7]1([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:19]2[CH:18]=[C:17]3[CH:20]([OH:24])[CH:21]([CH3:23])[CH2:22][C:16]3=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]

참가 물질

5

반응물 3

HCID 702EthanolHCID 4311764Sodium borohydrideHCID 71089296HCID 71089296, 화합물

생성물 1

HCID 71089357HCID 71089357, 화합물수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a 1000 mL round flask, 9,9-dihexyl-2-methyl-2,3-dihydrocyclopenta[b]fluoren-1(9H)-one (85 g, 211.1 mmol) was dissolved in 400 mL of THF and 400 mL of ethanol and then stirred. Sodium borohydride (NaBH4) (10 g, 265.0 mmol) was added to the reactant in five lots, and then stirred for 12 hours. After removal of the solvent, the resultant material was dissolved in ethylacetate, and then washed with water three times. The organic layer was dried over magnesium sulfate, followed by removal of volatile materials and drying, thereby obtaining 82.0 g of 9,9-dihexyl-2-methyl-1,2,3,9-tetrahydrocyclopenta[b]fluoren-1-ol (yield: 96.0%) (two isomers) as highly viscous oil.

후처리

  1. customAfter removal of the solvent
  2. dissolutionthe resultant material was dissolved in ethylacetate
  3. washwashed with water three times
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customfollowed by removal of volatile materials
  6. customdrying

출처 및 근거

ORD 기록
ord-4717ca9044804b2abe717be675f0beae
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394388B2

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