Hydrochloric Acid → HCID 66990811, 화합물

HRID 444628노트

반응식

HRID 444628 반응식
C[O:2][C:3]([C:5]1[C:6]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:16][C:15]=2[O:28][CH3:29])=[CH:7][CH:8]=[C:9]([C:11](=[O:13])[CH3:12])[CH:10]=1)=[O:4].[OH-].[Na+].CO.Cl>O>[C:11]([C:9]1[CH:10]=[C:5]([C:3]([OH:4])=[O:2])[C:6]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:16][C:15]=2[O:28][CH3:29])=[CH:7][CH:8]=1)(=[O:13])[CH3:12]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 66990886HCID 66990886, 화합물

생성물 1

HCID 66990811HCID 66990811, 화합물수율 74%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 4-Acetyl-4′-benzyloxy-2′-methoxybiphenyl-2-carboxylic acid methyl ester 7b (4.06 g, 9.7 mmol) and NaOH (0.773 g, 19.4 mmol) was added methanol (60 mL) and water (60 mL). The reaction was refluxed under Ar for 7 h then cooled to room temperature. After placing in an ice bath, 1 M HCl was added to give a yellow precipitate that was filtered, washed with water and recrystallized from THF/hexanes to give 2.7 g (69%) of 8b as yellow crystals. 1H-NMR (400 MHz, CDCl3) dH 2.68 (4H, s, COCH3), 3.62 (3H, s, OCH3), 5.16 (2H, s, CH2Ph), 6.77 (1H, s, ArH), 7.18 (1H, s, ArH), 7.33-7.52 (5H, m, CH2Ph), 3.90 (3H, s, OCH3), 5.22 (2H, S, CH2Ph), 6.58 (1H, s, ArH), 6.90 (1H, s, ArH), 7.34-7.50 (6H, m, ArH+Ch2Ph), 8.17 (1H, d, ArH), 8.50 (1H, s, ArH),

후처리

  1. temperatureThe reaction was refluxed under Ar for 7 h
  2. customAfter placing in an ice bath
  3. customto give a yellow precipitate that
  4. filtrationwas filtered
  5. washwashed with water
  6. customrecrystallized from THF/hexanes

출처 및 근거

ORD 기록
ord-64d49c6813b044379bed289f5b9607d6
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08475776B2

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