Sodium Chloride → {1-[(Benzyloxy)methyl]cyclobutyl}methyl methanesulfonate

HRID 1180764노트

반응식

HRID 1180764 반응식
[CH2:1]([O:8][CH2:9][C:10]1([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25].[Cl-].[Na+]>ClCCl>[CH3:23][S:24]([O:15][CH2:14][C:10]1([CH2:9][O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:11][CH2:12][CH2:13]1)(=[O:26])=[O:25]

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 11458402(1-((Benzyloxy)methyl)cyclobutyl)methanol

생성물 1

HCID 11346646{1-[(Benzyloxy)methyl]cyclobutyl}methyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 12.0 g (59.0 mmol) of {1-[(benzyloxy)methyl]cyclobutyl}methanol in 180 mL of dichloromethane was added 9.93 ml (70.8 mmol) of triethylamine at 0° C. followed by the addition of 5.02 mL (64.9 mmol) of methanesulfonyl chloride. After stirring for 2 h, saturated sodium chloride solution was added. The organic phase was isolated, dried using magnesium sulfate, and concentrated under vacuum to afford the crude product, which was used directly in the next step. 1H NMR (300 MHz, CDCl3) δ 7.39-7.32 (m, 5H), 4.57 (s, 2H), 4.30 (s, 2H), 3.52 (s, 2H), 2.98 (s, 3H), 1.95 (m, 6H).

후처리

  1. customThe organic phase was isolated
  2. customdried
  3. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-14527ff28ba54ae0a76ac68d373da9ec
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07282512B2

반응 노트

불러오는 중…