Lithium amide → 2,2,6,6-Tetramethyl-4-piperidinyl t-butyl-sulphonyl-acetate

HRID 26183

反応式

HRID 26183 の反応式
[C:1]([S:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])(=[O:7])=[O:6])([CH3:4])([CH3:3])[CH3:2].OC1[CH2:19][C:18]([CH3:21])([CH3:20])[NH:17][C:16]([CH3:23])([CH3:22])[CH2:15]1.[NH2-].[Li+]>C1(C)C(C)=CC=CC=1>[C:1]([S:5]([CH2:8][C:9]([O:11][CH:12]1[CH2:19][C:18]([CH3:21])([CH3:20])[NH:17][C:16]([CH3:23])([CH3:22])[CH2:15]1)=[O:10])(=[O:7])=[O:6])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 24532Lithium amideHCID 754714-Hydroxy-2,2,6,6-tetramethylpiperidineHCID 43444477Methyl 2-(2-methylpropane-2-sulfonyl)acetate

生成物 1

HCID 543326382,2,6,6-Tetramethyl-4-piperidinyl t-butyl-sulphonyl-acetate

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

実験手順

38.8 g (0.2 mol) of methyl t-butylsulphonyl-acetate, prepared according to the method of von Leusen and Strating, Rec. Trav, Chim. 84, 140 (1965), and 31.4 g (0.2 mol) of 4-hydroxy-2,2,6,6-tetramethylpiperidine are dissolved in 50 ml of xylene. The mixture is warmed to 130°, 0.2 g of lithium amide in 50 ml of xylene is added and the mixture is stirred for 12 hours at 130°-140°. The xylene is removed in vacuo and the residue is distilled to give 2,2,6,6-tetramethyl-4-piperidinyl t-butyl-sulphonyl-acetate; yield: 33.7 grams, boiling point 153°-154°/10-3 mm Hg.

後処理

  1. temperatureThe mixture is warmed to 130°
  2. customThe xylene is removed in vacuo
  3. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-e699c697c18f4bd396844235484c158f
出典データセット
uspto-grants-1979_04
特許番号
US04148784

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