p-Toluenesulfonic acid → HCID 69600972, 화합물

HRID 2215088노트

반응식

HRID 2215088 반응식
[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[N:14])[C@@H:5]([CH2:15][O:16]C2CCCCO2)[CH2:4][S:3]1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(N(CC)CC)C>CCO>[OH:16][CH2:15][C@H:5]1[CH2:4][S:3][C:2](=[O:1])[N:6]1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[N:14]

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 8471TriethylamineHCID 69601148HCID 69601148, 화합물

생성물 1

HCID 69600972HCID 69600972, 화합물수율 89.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 4-1 (0.97 g, 3.0 mmol) in 10 mL EtOH was added p-toluene sulfonic acid (50 mg) and the resulting solution was stirred overnight at room temperature. Triethylamine (0.1 mL) was added and the solution was concentrated in vacuo. The compound was purified by flash chromatography using 50–80% EtOAc/hexanes to yield 0.65 g of 4-2 as a colorless oil. 1H NMR (400 MHz, CDCl3): δ 3.92–3.73 (m, 3H), 3.68–3.60 (m, 1H), 3.42 (dd, 1H), 3.28 (dd, 1H), 3.10 (m, 1H), 2.37(t, 2H), 1.71–1.46 (m, 6H), 1.39–1.33 (m, 2H); MS (+ESI): m/z 243.1 (M+1)+.

후처리

  1. concentrationthe solution was concentrated in vacuo
  2. customThe compound was purified by flash chromatography

출처 및 근거

ORD 기록
ord-6ec3c79fb50d4fe089e24f14dc468379
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07109223B2

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