Triethylamine → HCID 178471604、化合物

HRID 26128ノート

反応式

HRID 26128 の反応式
C(N(CC)CC)C.Cl.[NH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].Cl[C:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[S:21](=[O:29])(=[O:28])[N:20]=1>O1CCOCC1>[O:28]=[S:21]1(=[O:29])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[C:19]([NH:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:20]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 64783Pseudosaccharin chlorideHCID 126496614-Aminobutyrate ethyl hydrochloride

生成物 1

HCID 178471604HCID 178471604、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

4.07 ml (29.2 mM) of triethylamine is added to 5.0 g. (29.2 mM) of ethyl 4-aminobutyrate hydrochloride, suspended in 75 ml of dioxane. After stirring for 5 minutes, 5.88 g. (29.2 mM) of 3-chloro-1,2-benzisothiazole 1,1-dioxide is added and the mixture is refluxed for one hour. The solvent is evaporated in vacuo and the residue is taken up in chloroform, washed with water, and evaporated to dryness. The residual 4-[(1,1-dioxo-1,2-benzisothiazol-3-yl)amino]-butanoic acid, ethyl ester is recrystallized from 40 ml. of methanol/water, yield 3.72 g., m.p. 125°-127°.

後処理

  1. temperaturethe mixture is refluxed for one hour
  2. customThe solvent is evaporated in vacuo
  3. washwashed with water
  4. customevaporated to dryness
  5. customThe residual 4-[(1,1-dioxo-1,2-benzisothiazol-3-yl)amino]-butanoic acid, ethyl ester is recrystallized from 40 ml

出典と根拠

ORDレコード
ord-2073cfa5dfc644b1b7a11fd14d15da28
出典データセット
uspto-grants-1979_04
特許番号
US04148798

反応ノート

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