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Hydrazine hydrate (1:1) → 1-Amino-3-(2,2,2-trifluoroethyl)-1,3-diazinan-2-one

HRID 63837
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HRID 63837 반응식
Cl[CH2:2][CH2:3][CH2:4][N:5]([CH2:15][C:16]([F:19])([F:18])[F:17])[C:6](=O)[O:7]C1C=CC=CC=1.[NH2:20][NH2:21].O>C(O)C>[NH2:20][N:21]1[CH2:2][CH2:3][CH2:4][N:5]([CH2:15][C:16]([F:19])([F:18])[F:17])[C:6]1=[O:7]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 118046857Phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate

생성물 1

HCID 1180467991-Amino-3-(2,2,2-trifluoroethyl)-1,3-diazinan-2-one

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
90 °C

실험 절차

Into a 100-mL round-bottom flask, was placed phenyl N-(3-chloropropyl)-N-(2,2,2-trifluoroethyl)carbamate (1.4 g, 4.73 mmol, 1.00 equiv), NH2NH2.H2O (6 mL), ethanol (40 mL). The resulting solution was stirred for 5 h at 90° C. in an oil bath. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 50 mL of H2O. The resulting solution was extracted with 3×30 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 2×30 mL of brine. The mixture was dried over anhydrous sodium sulfate. The resulting mixture was concentrated under vacuum. This resulted in 200 mg (crude) of 1-amino-3-(2,2,2-trifluoroethyl)-1,3-diazinan-2-one as a light yellow solid.

후처리

  1. customInto a 100-mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. additionThe resulting solution was diluted with 50 mL of H2O
  4. extractionThe resulting solution was extracted with 3×30 mL of ethyl acetate
  5. washThe resulting mixture was washed with 2×30 mL of brine
  6. dry with materialThe mixture was dried over anhydrous sodium sulfate
  7. concentrationThe resulting mixture was concentrated under vacuum
  8. customThis resulted in 200 mg (crude) of 1-amino-3-(2,2,2-trifluoroethyl)-1,3-diazinan-2-one as a light yellow solid

출처 및 근거

ORD 기록
ord-8cf40a6d89624d458983a906c0185f2d
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09447084B2

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