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Sulfuric Acid → HCID 70209846, 화합물

HRID 987333
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HRID 987333 반응식
[F:1][C:2]([F:8])([F:7])[CH:3]([CH3:6])[CH:4]=O.S(=O)(=O)(O)O.Cl.[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][O:24][C:25]2[CH:30]=[CH:29][C:28]([CH2:31][C@H:32]([O:36][CH2:37][CH3:38])[C:33]([OH:35])=[O:34])=[CH:27][CH:26]=2)=[CH:18][CH:17]=1.[BH4-].[Na+]>O1CCCC1.ClCCl.CO>[CH2:37]([O:36][C@@H:32]([CH2:31][C:28]1[CH:29]=[CH:30][C:25]([O:24][CH2:23][CH2:22][C:19]2[CH:20]=[CH:21][C:16]([NH:15][CH2:4][CH:3]([CH3:6])[C:2]([F:8])([F:7])[F:1])=[CH:17][CH:18]=2)=[CH:26][CH:27]=1)[C:33]([OH:35])=[O:34])[CH3:38]
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참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 27821883,3,3-trifluoro-2-methylpropanalHCID 4311764Sodium borohydrideHCID 86595065HCID 86595065, 화합물

생성물 1

HCID 70209846HCID 70209846, 화합물수율 54.1%

시약·촉매·용매 3

HCID 887Methanol용매
HCID 6344
Dichloromethane
용매
HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

2-(Trifluoromethyl)propionaldehyde (0.0724 g; 0.574 mmole) was dissolved in tetrahydrofurane (3 ml) and sulfuric acid (4 M; 0.041 ml; 0.164 mmole) was added under stirring, followed by addition of 3-{4-[2-(4-aminophenyl)ethoxy]phenyl}-(S)-2-ethoxypropanoic acid hydro chloride (described in Example 56a) (0.2 g; 0.547 mmole) dissolved in tetrahydrofurane (2 ml). The reaction mixture was stirred for 10 minutes, then cooled to 0° C in an ice-bath and sodium borohydride (0.042 g; 1.10 mmole) was added. After addition, the cooling bath was removed. The mixture was stirred overnight and then evaporated to remove tetrahydrofurane. Ethyl acetate and water were added into the residue and the organic phase was separated, washed with brine, dried with magnesium sulfate. The solvent was then evaporated. Chromatography on silica gel(Isolute, SI ) using dichloromethane and then 1% methanol in dichloromethane as eluant gave 0.13 g (40% yield) of (S)-2-ethoxy-3-(4-{2-[4-(3,3,3-trifluoro-2-methyl-(R/S)-propylamino)phenyl]ethoxy}phenyl)propanoic acid.

후처리

  1. stirringThe reaction mixture was stirred for 10 minutes
  2. additionAfter addition
  3. customthe cooling bath was removed
  4. stirringThe mixture was stirred overnight
  5. customevaporated
  6. customto remove tetrahydrofurane
  7. additionEthyl acetate and water were added into the residue
  8. customthe organic phase was separated
  9. washwashed with brine
  10. dry with materialdried with magnesium sulfate
  11. customThe solvent was then evaporated

출처 및 근거

ORD 기록
ord-41bdc8b91dfc4e8eb0437f61bfc6f5ce
출처 데이터셋
uspto-grants-2003_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06630600B1

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