Borane;tetrahydrofuran → (3-Chloropropyl)(2,2,2-trifluoroethyl)amine

HRID 63835노트

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HRID 63835 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][NH:5][C:6](=O)[C:7]([F:10])([F:9])[F:8].B.C1COCC1>O1CCCC1>[Cl:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][C:7]([F:10])([F:9])[F:8]

참가 물질

4

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온도
80 °C

실험 절차

Into a 250-mL round-bottom flask, was placed N-(3-chloropropyl)-2,2,2-trifluoroacetamide (6 g, 31.65 mmol, 1.00 equiv), tetrahydrofuran (30 mL), BH3/THF (80 mL). The resulting solution was stirred for 3 h at 80° C. in an oil bath. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 200 mL of H2O. The resulting solution was extracted with 4×100 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 2×100 mL of brine. The mixture was dried over anhydrous sodium sulfate. This resulted in 5 g (90%) of (3-chloropropyl)(2,2,2-trifluoroethyl)amine as a light yellow liquid.

후처리

  1. customInto a 250-mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. additionThe resulting solution was diluted with 200 mL of H2O
  4. extractionThe resulting solution was extracted with 4×100 mL of ethyl acetate
  5. washThe resulting mixture was washed with 2×100 mL of brine
  6. dry with materialThe mixture was dried over anhydrous sodium sulfate
  7. customThis resulted in 5 g (90%) of (3-chloropropyl)(2,2,2-trifluoroethyl)amine as a light yellow liquid

출처 및 근거

ORD 기록
ord-e7bd272bccab47cd996ea45e00d8bdd3
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447084B2

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