Triethylamine → HCID 68686408, 화합물

HRID 1442677노트

반응식

HRID 1442677 반응식
Cl.[CH3:2][O:3][C:4](=[O:7])[CH2:5][NH2:6].CCN(CC)CC.[CH:15]1([CH2:18][O:19][C:20]2[CH:25]=[CH:24][C:23]([S:26](Cl)(=[O:28])=[O:27])=[CH:22][CH:21]=2)[CH2:17][CH2:16]1>O1CCOCC1.O>[CH3:2][O:3][C:4](=[O:7])[CH2:5][NH:6][S:26]([C:23]1[CH:22]=[CH:21][C:20]([O:19][CH2:18][CH:15]2[CH2:16][CH2:17]2)=[CH:25][CH:24]=1)(=[O:28])=[O:27]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 122755Glycine methyl ester hydrochlorideHCID 113686084-(cyclopropylmethoxy)benzenesulfonyl Chloride

생성물 1

HCID 68686408HCID 68686408, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of 7.125 g (56.75 mmol) of glycine methylester hydrochloride in 60 ml of dioxane and 24 ml of H2O, 15 ml (107.8 mmol) of Et3N and then a solution of 10 g (40.53 mmol) of 4-cyclopropylmethoxy-benzenesulfonyl chloride in 10 ml of dioxane are added dropwise at 0-5° C. After stirring for 3 h at r.t., the reaction is quenched with ice water and the mixture is extracted with AcOEt. The combined extracts are washed with H2O, brine, dried over MgSO4 and concentrated under reduced pressure to give the title compound as a colorless solid; 1H-NMR (400MHz, CDCl3): 0.3-0.40 (m, 2H), 0.65-0.72 (m, 2H), 1.20-1.35 (m, 1H), 3.65 (m, 3H), 3.77 (d, 2H, J=5.04 Hz), 3.86 (d, 2H, J=7.08 Hz), 4.98 (brs, 1H), 6.96 (d, 2H, J=8.52 Hz), 7.77 (d, 2H, J8.52 Hz).

후처리

  1. customthe reaction is quenched with ice water
  2. extractionthe mixture is extracted with AcOEt
  3. washThe combined extracts are washed with H2O, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-28abe593af2c48369c4a1dbb5fca18a5
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07659293B2

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