Hydrochloric Acid → HCID 19896683, 화합물

HRID 1196863

반응식

HRID 1196863 반응식
[NH:1]1[CH2:6][CH2:5][S:4][CH2:3][CH:2]1[C:7]([O:9][CH2:10][CH3:11])=[O:8].C(N(CC)CC)C.[C:19]1([CH3:31])[CH:24]=[C:23]([CH3:25])[CH:22]=[C:21]([CH3:26])[C:20]=1[CH2:27][C:28](Cl)=[O:29].Cl>O.C1COCC1>[CH3:31][C:19]1[CH:24]=[C:23]([CH3:25])[CH:22]=[C:21]([CH3:26])[C:20]=1[CH2:27][C:28]([N:1]1[CH2:6][CH2:5][S:4][CH2:3][CH:2]1[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:29]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 110307542,4,6-Trimethylbenzeneacetyl chlorideHCID 13604869Ethyl thiomorpholine-3-carboxylate

생성물 1

HCID 19896683HCID 19896683, 화합물수율 94.7%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

175.3 g (1 mol) of ethyl thiomorpholine-3-carboxylate are dissolved in 1000 ml of abs. THF, 140 ml (1 mol) of triethylamine are added and 198.5 g (1 mol) of mesitylene acetyl chloride are added dropwise at 0° to 10° C. The mixture is subsequently stirred at room temperature for a further 1 h and poured into 4.5 1 of ice water and 500 ml of 1 N HCl, and a flocculant, strongly water-containing product is filtered off with suction, taken up in methylene chloride, dried using MgSO4 and concentrated on a rotary evaporator. In this manner, 317.2 g (=94.7% of theory) of ethyl N-(2,4,6-trimethylphenyl-acetyl)-thiomorpholine-3-carboxylate are obtained as a pale yellow oil.

후처리

  1. filtrationis filtered off with suction
  2. customdried
  3. concentrationconcentrated on a rotary evaporator

출처 및 근거

ORD 기록
ord-220b73f5198c4dcfbfad3c7165d31af5
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05116836

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