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Lithium Hydroxide → 3-Benzyloxy-5-isopropyl-thiophene-2-carboxylic acid

HRID 1445332
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HRID 1445332 반응식
[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([CH:14]([CH3:16])[CH3:15])[S:11][C:10]=1[C:17]([O:19]C)=[O:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Li+]>O1CCCC1.CO.O>[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([CH:14]([CH3:16])[CH3:15])[S:11][C:10]=1[C:17]([OH:19])=[O:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

6

반응물 2

HCID 3939Lithium HydroxideHCID 21961236Methyl 3-benzyloxy-5-isopropyl-thiophene-2-carboxylate

생성물 1

HCID 219612383-Benzyloxy-5-isopropyl-thiophene-2-carboxylic acid

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

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온도
22 °C

실험 절차

1.16 g of methyl 3-benzyloxy-5-isopropyl-thiophene-2-carboxylate were dissolved in 10 ml of tetrahydrofuran (THF) and 10 ml of methanol, and a solution of 1.7 g of lithium hydroxide in 10 ml of water was added. The reaction mixture was stirred at 22° C. for 72 h. Methanol and THF were stripped off in the rotary evaporator. While cooling in ice, the reaction mixture was adjusted to pH=4 with 2 molar hydrochloric acid and extracted twice with 50 ml of ethyl acetate each time. The combined organic phases were dried over sodium sulfate and concentrated.

후처리

  1. customMethanol and THF were stripped off in the rotary evaporator
  2. temperatureWhile cooling in ice
  3. extractionextracted twice with 50 ml of ethyl acetate each time
  4. dry with materialThe combined organic phases were dried over sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-969aa52c14c049f7bfb67d773daa699d
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07666848B2

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