O-[(5-chlorothiophen-2-yl)methyl]hydroxylamine → HCID 136127206, 화합물

HRID 621370노트

반응식

HRID 621370 반응식
[C:1]([C:4]1[C:5](=[O:17])[CH2:6][CH:7]([CH:11]2[CH2:16][CH2:15][CH2:14][S:13][CH2:12]2)[CH2:8][C:9]=1[OH:10])(=O)[CH3:2].[Cl:18][C:19]1[S:23][C:22]([CH2:24][O:25][NH2:26])=[CH:21][CH:20]=1>C(O)C>[Cl:18][C:19]1[S:23][C:22]([CH2:24][O:25][N:26]=[C:1]([C:4]2[C:5](=[O:17])[CH2:6][CH:7]([CH:11]3[CH2:16][CH2:15][CH2:14][S:13][CH2:12]3)[CH2:8][C:9]=2[OH:10])[CH3:2])=[CH:21][CH:20]=1

참가 물질

4

반응물 2

HCID 10986580O-[(5-chlorothiophen-2-yl)methyl]hydroxylamineHCID 15614621HCID 15614621, 화합물

생성물 1

HCID 136127206HCID 136127206, 화합물수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution containing 5.1 g (0.020 mol) of 2-acetyl-3-hydroxy-5-(tetrahydro-2H-thiopyran-3-yl)cyclohex-2-en-1-one and 3.4 g (0.021 mol) of (5-chlorothien-2-yl)methoxyamine in 200 ml of ethanol was stirred overnight (about 14 hours) at room temperature and then evaporated to remove ethanol. The concentrate was diluted with 150 ml of methylene chloride and then washed with 100 ml of water and then with 100 ml of saturated aqueous sodium chloride solution. The washed methylene chloride solution was dried over anhydrous magnesium sulfate and then evaporated to dryness under reduced pressure to afford a white solid. Recrystallation of this solid with absolute ethanol afforded 7.6 g of the title compound, m.p. 154°-155° C. cl EXAMPLE 2

후처리

  1. customevaporated
  2. customto remove ethanol
  3. additionThe concentrate was diluted with 150 ml of methylene chloride
  4. washwashed with 100 ml of water
  5. dry with materialThe washed methylene chloride solution was dried over anhydrous magnesium sulfate
  6. customevaporated to dryness under reduced pressure
  7. customto afford a white solid

출처 및 근거

ORD 기록
ord-14a32d15285245cc88b0fdf6fbdb98ff
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824470

반응 노트

불러오는 중…