Acetyl chloride → HCID 58997658, 화합물

HRID 1592353

반응식

HRID 1592353 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][NH2:11])=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:19](Cl)(=[O:21])[CH3:20]>C1COCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][CH2:10][NH:11][C:19](=[O:21])[CH3:20])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 64837963-(4-Fluorophenyl)propan-1-amine

생성물 1

HCID 58997658HCID 58997658, 화합물수율 86.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

1-(para-fluorophenyl)-3-aminopropane (1.00 g, 6.53 mmol, 1 eq.) and triethylamine (0.91 mL, 6.53 mmol, 1 eq.) were dissoved in THF (10 mL) at 25° C. under N2. Then a THF solution (5 mL) of acetyl chloride (0.46 mL, 6.53 mmol, 1 eq.) was added dropwise via an addition funnel over 10 minutes. Worked up after 20 minutes by filtering off the solids then stripping the filtrate to obtain an amber oil. The oil was purified over silica gel in 1:1 Hexanes/EtOAc to 100% EtOAc to 4:1 EtOAc/MeOH. Obtained 1.10 g of an amber oil as product. MS (ESI) detects (M+H)+=196.

후처리

  1. filtrationby filtering off the solids
  2. customto obtain an amber oil
  3. customThe oil was purified over silica gel in 1:1 Hexanes/EtOAc to 100% EtOAc to 4:1 EtOAc/MeOH

출처 및 근거

ORD 기록
ord-97594fdb46f9489b82ad8fee77b8bec0
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07291744B2

연결된 노트

불러오는 중…