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Chloroacetyl chloride → HCID 86623719, 화합물

HRID 249854
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HRID 249854 반응식
Cl[CH2:2][C:3]([Cl:5])=[O:4].[CH2:6]([NH:13][C@H:14]([CH3:17])[CH2:15][OH:16])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:6]([NH:13][C@H:14]([CH3:17])[CH2:15][O:16][CH2:2][C:3]([Cl:5])=[O:4])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
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참가 물질

5

반응물 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 7353896(2R)-2-(benzylamino)propan-1-ol

생성물 1

HCID 86623719HCID 86623719, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Chloroacetyl chloride (11.6 mL, 120 mmol) was added dropwise at 0° C. to a solution of (R)-2-(benzylamino)propan-1-ol (19.9 g, 120 mmol) and triethylamine (30.5 mL) in toluene (600 mL). The cooling bath was removed and the reaction mixture was stirred at room temperature for 18 h. The reaction was concentrated under reduced pressure and the recovered solids dissolved in EtOAc (500 mL) and then washed with saturated bicarbonate (2×250 mL), H2O (250 mL) and saturated brine (250 mL). The organic phase was then dried (Na2SO4), filtered and concentrated to afford (R)-2-(2-(benzylamino)propoxy)acetyl chloride: MS consistent.

후처리

  1. customThe cooling bath was removed
  2. concentrationThe reaction was concentrated under reduced pressure
  3. dissolutionthe recovered solids dissolved in EtOAc (500 mL)
  4. washwashed with saturated bicarbonate (2×250 mL), H2O (250 mL) and saturated brine (250 mL)
  5. dry with materialThe organic phase was then dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3cd8fafccf3a42d8990799337093fa76
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863271B2

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