Lithium Hydroxide → 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid

HRID 1853949

反応式

HRID 1853949 の反応式
C[O:2][C:3](=[O:21])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[C:6]([N:11]2[CH2:20][CH2:19][C:14]3([O:18][CH2:17][CH2:16][O:15]3)[CH2:13][CH2:12]2)[CH:5]=1.[OH-].[Li+]>>[O:15]1[C:14]2([CH2:19][CH2:20][N:11]([C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=3[CH3:10])[C:3]([OH:21])=[O:2])[CH2:12][CH2:13]2)[O:18][CH2:17][CH2:16]1

参加物

3

反応物 2

HCID 3939Lithium HydroxideHCID 673546753-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid methyl ester

生成物 1

HCID 673566093-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid

実験手順

A solution of 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid methyl ester (100 mg, 0.343 mmol] in 3 ml of mixed solvent [1:0.3:0.5 THF/water/methanol] was treated with lithium hydroxide (12.25 mg, 0.514 mmol]. The reaction mixture was stirred at room temperature for 6 hours, concentrated and acidified [pH=4] with 2M HCl. The precipitate obtained was filtered, washed with water and dried under vacuum. The crude material was washed with ether, air dried overnight to give desired product. i.e., 3-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-4-methyl-benzoic acid [12] as yellow colored solid. On the basis of mass recovery (93.2 mg) the yield was assumed to be quantitative.

後処理

  1. concentrationconcentrated
  2. customThe precipitate obtained
  3. filtrationwas filtered
  4. washwashed with water
  5. customdried under vacuum
  6. washThe crude material was washed with ether, air
  7. customdried overnight

出典と根拠

ORDレコード
ord-4f29474499c7484c88e9823d1adea9ae
出典データセット
uspto-grants-2015_02
特許番号
US08962637B2

関連ノート

読み込み中…