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Sodium Hydroxide → 85795-31-9

HRID 1702193
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HRID 1702193 반응식
[CH3:1][N:2]1[C:6]([CH2:7][C:8]([O:10]C)=[O:9])=[CH:5][C:4]2[CH2:12][O:13][C:14]3[CH:21]=[C:20]([CH3:22])[CH:19]=[CH:18][C:15]=3[C:16](=[O:17])[C:3]1=2.[OH-].[Na+]>CO.O>[CH3:1][N:2]1[C:6]([CH2:7][C:8]([OH:10])=[O:9])=[CH:5][C:4]2[CH2:12][O:13][C:14]3[CH:21]=[C:20]([CH3:22])[CH:19]=[CH:18][C:15]=3[C:16](=[O:17])[C:3]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 13179849HCID 13179849, 화합물

생성물 1

HCID 1317985085795-31-9수율 90.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To an ice-cooled suspension of 1.74 g (0.006 m) of methyl 4,10-dihydro-1,7-dimethyl-10-oxo-1H[1]-benzoxepino[4,3-b]pyrrole-2-acetate in a mixture of methanol (50 ml) and water (5 ml) under a nitrogen atmosphere was added 2.5 N sodium hydroxide solution (2.6 cc, 0.0066 m) over 1 minute. After 30 minutes the ice-bath was removed, and the mixture stirred at ambient temperatures for five hours. The mixture was diluted to ca. 150 ml with water, aged, filtered, and the filtrate acidified dropwise with 2.0 N hydrochloric acid. After filtration, washing and drying, 1.5 g of product was obtained which upon recrystallization from i-propanol-water yielded pure 4,10-dihydro-1,7-dimethyl-10-oxo-1H[1]-benzoxepino[4,3-b]-pyrrole-2-acetic acid, m.p. 196°-197° C.

후처리

  1. customAfter 30 minutes the ice-bath was removed
  2. additionThe mixture was diluted to ca. 150 ml with water
  3. filtrationfiltered
  4. filtrationAfter filtration
  5. washwashing
  6. customdrying

출처 및 근거

ORD 기록
ord-5b9cb92948a042e7bb66fc8aa518e5a9
출처 데이터셋
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04380645

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