Potassium Hydroxide → HCID 86642595, 화합물

HRID 2421577

반응식

HRID 2421577 반응식
[Cl:1]C1C=CC2OC3C=CC=CC=3[C@H]3C(=[O:13])N(C)C[C@@H]3C=2C=1.[Cl:22][C:23]1[CH:24]=[CH:25][C:26]2[O:37][C:36]3[CH:38]=[CH:39][CH:40]=[CH:41][C:35]=3[C@@H:29]3[C:30](=[O:34])[N:31]([CH3:33])[CH2:32][C@@H:28]3[C:27]=2[CH:42]=1.[OH-].[K+]>C(O)C>[ClH:1].[Cl:22][C:23]1[CH:24]=[CH:25][C:26]2[O:37][C:36]3[CH:38]=[CH:39][CH:40]=[CH:41][C:35]=3[C@@H:29]([C:30]([OH:34])=[O:13])[C@H:28]([CH2:32][NH:31][CH3:33])[C:27]=2[CH:42]=1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 56960600912356-09-3HCID 58729182(3aS,12bS)-5-chloro-2-methyl-2,3,3a,12b-tetrahydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrol-1-one

생성물 1

HCID 86642595HCID 86642595, 화합물수율 22%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The mixture of lactams (VII) and (VIII) (13.6 grams, 45 mmol, trans/cis ratio 1:2.3), obtained as described under E, was dissolved in ethanol (140 ml). To the solution potassium hydroxide was added (43 grams, 811 mmol), whereupon the mixture was heated to reflux for 18 hours. Part of the ethanol (60 ml) was evaporated and water was added (200 mL). The aqueous phase was extracted twice with toluene (100 ml). Subsequently toluene (100 ml) was added to the water phase, followed by concentrated hydrochloric acid to adjust the pH to 1. During the addition of hydrochloric acid the temperature rises to 75° C. The water layer was separated and upon cooling the product crystallized. The crystals were collected by filtration and dried to provide trans-2-chloro-10,11-dihydro-11[(methylamino)methyl]-dibenz[b,f]oxepin-10-carboxylic acid hydrochloride (II) (3.75 grams, 10.6 mmol, 22%).

후처리

  1. customobtained
  2. temperaturewhereupon the mixture was heated
  3. temperatureto reflux for 18 hours
  4. customPart of the ethanol (60 ml) was evaporated
  5. additionwater was added (200 mL)
  6. extractionThe aqueous phase was extracted twice with toluene (100 ml)
  7. additionSubsequently toluene (100 ml) was added to the water phase
  8. additionDuring the addition of hydrochloric acid the temperature
  9. customrises to 75° C
  10. customThe water layer was separated
  11. temperatureupon cooling the product
  12. customcrystallized
  13. filtrationThe crystals were collected by filtration
  14. customdried

출처 및 근거

ORD 기록
ord-43fb4c6dadf14b0c8eea56b0c28b216a
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07956202B2

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