2-[(1-Methoxymethoxy-5,6,7,8-tetrahydro-naphthalene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester → HCID 57912188、化合物

HRID 238898ノート

反応式

HRID 238898 の反応式
[CH3:1][O:2][C:3](=[O:24])[C:4]([NH:7][C:8]([C:10]1[CH:19]=[CH:18][C:17]2[CH2:16][CH2:15][CH2:14][CH2:13][C:12]=2[C:11]=1[O:20]COC)=[O:9])([CH3:6])[CH3:5]>C(O)(C)C.O1CCCC1.Cl>[CH3:1][O:2][C:3](=[O:24])[C:4]([NH:7][C:8]([C:10]1[CH:19]=[CH:18][C:17]2[CH2:16][CH2:15][CH2:14][CH2:13][C:12]=2[C:11]=1[OH:20])=[O:9])([CH3:6])[CH3:5]

参加物

5

反応物 1

HCID 688409232-[(1-Methoxymethoxy-5,6,7,8-tetrahydro-naphthalene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester

生成物 1

HCID 57912188HCID 57912188、化合物収率 96.4%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 3776Isopropanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1.023 g 2-[(1-methoxymethoxy-5,6,7,8-tetrahydro-naphthalene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester was dissolved in a mixture of isopropanol (8 ml), tetrahydrofurane (8 ml) and HCl conc. (4 ml). It was stirred at room temperature for one hour. The mixture was concentrated in vacuo, then 20 ml of ethyl acetate and 30 ml of water were added to the residue. The organic layer was separated, dried over magnesium sulphate and concentrated in vacuo to afford 0.857 g of 2-[(1-hydroxy-5,6,7,8-tetrahydro-naphthalene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. addition20 ml of ethyl acetate and 30 ml of water were added to the residue
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3464ba9f4f3b44ca89f4693541e7cfb6
出典データセット
uspto-grants-2014_02
特許番号
US08642643B2

反応ノート

読み込み中…