Water → HCID 87416741, 화합물

HRID 600945노트

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HRID 600945 반응식
C[O:2][C:3](=[O:23])/[C:4](/[C:12]1[CH:17]=[CH:16][C:15]([S:18]([CH3:21])(=[O:20])=[O:19])=[C:14]([Cl:22])[CH:13]=1)=[N:5]/[O:6][CH:7]1[CH2:11][CH2:10][CH2:9][CH2:8]1.[OH-].[Li+].O>CO.C(Cl)(Cl)Cl>[Cl:22][C:14]1[CH:13]=[C:12](/[C:4](=[N:5]\[O:6][CH:7]2[CH2:11][CH2:10][CH2:9][CH2:8]2)/[C:3]([OH:23])=[O:2])[CH:17]=[CH:16][C:15]=1[S:18]([CH3:21])(=[O:20])=[O:19]

참가 물질

6

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 87416800methyl (2E)-2-(3-chloro-4-methylsulfonylphenyl)-2-cyclopentyloxyiminoacetate

생성물 1

HCID 87416741HCID 87416741, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

(E)-(3-Chloro-4-methanesulfonyl-phenyl)-cyclopentyloxyimino-acetic acid methyl ester (144 mg, 0.40 mmol) was dissolved in methanol (4 mL) and cooled in an ice bath. A 2.0 N solution of lithium hydroxide in water (0.60 mL, 1.2 mmol) was added dropwise. After stirring 1 h, the reaction mixture was diluted with chloroform (50 mL) and washed with 0.1 M aqueous potassium bisulfate (25 mL). The aqueous phase was extracted with chloroform (30 mL) and the combined organic phases were dried over magnesium sulfate and evaporated in vacuo to afford (E)-(3-chloro-4-methanesulfonyl-phenyl)-cyclopentyloxyimino-acetic acid which was used in the next step without further purification: H1-NMR (400 MHz, CDCl3) δ=1.65 (4H, m), 1.88 (4H, m), 3.31 (3H, s), 4.97 (1H, m), 7.58 (1H, dd, J=8.2 Hz, J=1.1 Hz), 7.67 (1H, d, J=1.1 Hz), 8.19 (1H, d, J=8.2 Hz).

후처리

  1. temperaturecooled in an ice bath
  2. washwashed with 0.1 M aqueous potassium bisulfate (25 mL)
  3. extractionThe aqueous phase was extracted with chloroform (30 mL)
  4. dry with materialthe combined organic phases were dried over magnesium sulfate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-93ac6b35d6474007821a7cc503a93a59
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902248B2

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