홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Chlorotrimethylsilane → 2-Amino-4,4,4-trifluorobutan-1-ol

HRID 1365550
노트
인쇄 미리보기

반응식

HRID 1365550 반응식
[Li+].[BH4-].C[Si](Cl)(C)C.[NH2:8][CH:9]([CH2:13][C:14]([F:17])([F:16])[F:15])[C:10](O)=[O:11]>C1COCC1>[NH2:8][CH:9]([CH2:13][C:14]([F:17])([F:16])[F:15])[CH2:10][OH:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 3530832-Amino-4,4,4-trifluorobutanoic acidHCID 4148881Lithium borohydride

생성물 1

HCID 534164332-Amino-4,4,4-trifluorobutan-1-ol수율 53.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of LiBH4 (62.7 mg, 2.88 mmol) in THF (1.5 mL) was added TMSCl (728 μL, 5.76 mmol) and the reaction mixture was stirred at room temperature for 15 min, followed by the addition of 2-amino-4,4,4-trifluorobutanoic acid (226 mg, 1.44 mmol). The reaction mixture was stirred at room temperature for 18 h, and quenched by careful addition of MeOH. The solvents were removed by reduced pressure, and to the residue was added H2O (2.08 mL). The resulting aqueous portion was made basic by adding 2 N NaOH. The mixture was extracted with CH2Cl2 three times. The combined organic portions were dried over MgSO4, filtered and concentrated to give 2-amino-4,4,4-trifluorobutan-1-ol as a colorless oil (110 mg, 53% yield). NMR: 400 MHz 1H (CDCl3) 3.61 ppm, 1 H, dd, J=10.61, 4.04 Hz; 3.42 ppm, 1 H, m; 3.28 ppm, 1 H, m; 2.29 ppm, 1 H, m; 2.12 ppm, 1 H, m.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 18 h
  2. customquenched by careful addition of MeOH
  3. customThe solvents were removed by reduced pressure
  4. additionto the residue was added H2O (2.08 mL)
  5. additionby adding 2 N NaOH
  6. extractionThe mixture was extracted with CH2Cl2 three times
  7. dry with materialThe combined organic portions were dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-401086c64e2c4d21b2e5e4d4ece259c1
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07888376B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트