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Sulfamic Acid → 4-Methoxy-indan-5-carboxylic acid

HRID 389323
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반응식

HRID 389323 반응식
[CH3:1][O:2][C:3]1[C:11]([CH:12]=[O:13])=[CH:10][CH:9]=[C:8]2[C:4]=1[CH2:5][CH2:6][CH2:7]2.S(=O)(=O)([OH:16])N.Cl([O-])=O.[Na+]>ClCCl.O>[CH3:1][O:2][C:3]1[C:11]([C:12]([OH:16])=[O:13])=[CH:10][CH:9]=[C:8]2[C:4]=1[CH2:5][CH2:6][CH2:7]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 5987Sulfamic AcidHCID 23668197Sodium ChloriteHCID 866431044-Methoxy-indan-5-carbaldehyde

생성물 1

HCID 668121244-Methoxy-indan-5-carboxylic acid수율 96%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6344Dichloromethane용매
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반응 조건

온도
26.5 °C

실험 절차

To a clear solution of 4-Methoxy-indan-5-carbaldehyde (11.5 gm, 0.065 mole) in Dichloromethane (100 ml), Sulphamic acid (19.0 gm, 0.196 mole) was added at 25-28°. A solution of Sodium chlorite (15.28 gm, 0.169 mole) in water (50 ml) was added at 5-10° C. The reaction mixture was stirred for 5 hours at 25-28° C. Finally the reaction mixture was poured into water (200 ml) and extracted with Dichloromethane (2×200 ml). The organic layer was dried over Sodium sulphate, distilled under vacuum to give 12.0 gm of desired product as a viscous oil.

후처리

  1. extractionextracted with Dichloromethane (2×200 ml)
  2. dry with materialThe organic layer was dried over Sodium sulphate
  3. distillationdistilled under vacuum

출처 및 근거

ORD 기록
ord-82fc4be876ee41f49202107458527c45
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08378118B2

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