Hydrochloric Acid → 4'-Methyl-5-(5-oxa-6-azaspiro[3.4]oct-6-en-7-yl)biphenyl-3-carboxylic acid

HRID 1257551노트

반응식

HRID 1257551 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[C:12]([C:14]3[CH2:21][C:17]4([CH2:20][CH2:19][CH2:18]4)[O:16][N:15]=3)[CH:11]=[C:10]([C:22]([O:24]C(C)(C)C)=[O:23])[CH:9]=2)=[CH:4][CH:3]=1.Cl>ClCCl>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[C:12]([C:14]3[CH2:21][C:17]4([CH2:18][CH2:19][CH2:20]4)[O:16][N:15]=3)[CH:11]=[C:10]([C:22]([OH:24])=[O:23])[CH:9]=2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66895976Tert-butyl 4'-methyl-5-(5-oxa-6-azaspiro[3.4]oct-6-en-7-yl)biphenyl-3-carboxylate

생성물 1

HCID 668957974'-Methyl-5-(5-oxa-6-azaspiro[3.4]oct-6-en-7-yl)biphenyl-3-carboxylic acid수율 93.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 4′-methyl-5-(5-oxa-6-azaspiro[3.4]oct-6-en-7-yl)biphenyl-3-carboxylate (1.26 g, 3.34 mmol) in dichloromethane (12 mL) was added hydrogen chloride (4.0 M in dioxane; 4.17 mL, 16.7 mmol). The reaction mixture was stirred at ambient temperature. After 18 h, the mixture was concentrated. Dichloromethane was added and the suspension was filtered. The solid cake was washed with dihchloromethane and dried under reduced pressure gave the title compound (1.0 g). MS 322.2 (M+1).

후처리

  1. concentrationthe mixture was concentrated
  2. additionDichloromethane was added
  3. filtrationthe suspension was filtered
  4. washThe solid cake was washed with dihchloromethane
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-a840c02afe6f405d80f373de8b4de5aa
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461185B2

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