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Potassium Hydroxide → Ro 40-6055

HRID 2076424
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HRID 2076424 반응식
[CH3:1][C:2]1([CH3:27])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]([NH:16][C:17]3[CH:26]=[CH:25][C:20]([C:21]([O:23]C)=[O:22])=[CH:19][CH:18]=3)=[O:15])[CH:5]=[CH:4][C:3]1=2.[OH-].[K+]>CO>[CH3:1][C:2]1([CH3:27])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]2[CH:7]=[C:6]([C:14]([NH:16][C:17]3[CH:18]=[CH:19][C:20]([C:21]([OH:23])=[O:22])=[CH:25][CH:26]=3)=[O:15])[CH:5]=[CH:4][C:3]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 13655816HCID 13655816, 화합물

생성물 1

HCID 2126Ro 40-6055수율 78.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 25 mL round bottom flask equipped with a reflux condenser was charged with methyl methyl 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-carboxamido)benzoate 3 (0.200 g, 0.547 mmol), MeOH (10 mL) and KOH (0.122 g, 2.18 mmol). The reaction mixture was stirred for 16 h at reflux, evaporated to dryness and partitioned between EtOAc and H2O. 6N HCl was added until pH became acidic and the organic layer was separated, washed with water, brine, dried with Na2SO4, filtered and concentrated on a rotary evaporator to give 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-carboxamido)benzoic acid 4 as a white solid (0.151 g, 78%).

후처리

  1. customA 25 mL round bottom flask equipped with a reflux condenser
  2. temperatureat reflux
  3. customevaporated to dryness
  4. custompartitioned between EtOAc and H2O
  5. addition6N HCl was added until pH
  6. customthe organic layer was separated
  7. washwashed with water, brine
  8. dry with materialdried with Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated on a rotary evaporator

출처 및 근거

ORD 기록
ord-ce56633a077b43f5ac345be186b4e856
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07923579B2

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