Sodium borohydride → HCID 71089357, 화합물

HRID 2273375노트

반응식

HRID 2273375 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].[BH4-].[Na+]>C1COCC1.C(O)C>[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 2

HCID 4311764Sodium borohydrideHCID 71089296HCID 71089296, 화합물

생성물 1

HCID 71089357HCID 71089357, 화합물수율 96%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 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 THF 400 mL and ethanol 400 mL, and then stirred. Sodium borohydride (NaBH4) (10 g, 265.0 mmol) was added to the reaction product in five lots, and then stirred for 12 hours. The resultant mixture, after removal of solvent, 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, to thereby obtain 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. customThe resultant mixture, after removal of solvent
  2. dissolutionwas 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-7b4a6be3fd84430c8523ec0cb7f14e62
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09120884B2

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