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

HRID 1257551ノート

反応式

HRID 1257551 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a840c02afe6f405d80f373de8b4de5aa
出典データセット
uspto-grants-2013_06
特許番号
US08461185B2

反応ノート

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