Acetyl chloride → HCID 2825757、化合物

HRID 867427ノート

反応式

HRID 867427 の反応式
[CH3:1][C:2]1([CH3:16])[S:6][C@@H:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[NH:4][C@H:3]1[C:13]([OH:15])=[O:14].[C:17](Cl)(=[O:19])[CH3:18]>N1C=CC=CC=1>[C:17]([N:4]1[C@@H:3]([C:13]([OH:15])=[O:14])[C:2]([CH3:16])([CH3:1])[S:6][C@H:5]1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:19])[CH3:18]

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 14548321HCID 14548321、化合物

生成物 1

HCID 2825757HCID 2825757、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

0.47 g (2 mmoles) of 5,5-dimethyl-2(S)-phenylthiazolidine-4(S)-carboxylic acid is suspended in 5 ml of pyridine while stirring. The temperature of the suspension is adjusted to 5° C. by cooling with ice-water and 0.17 g of acetyl chloride is dropped in. The mixture is stirred for 1 additional hour, then poured in 60 ml of ice-cold 2N sulphuric acid. After several hours, the precipitated product is filtered out, washed with water and dried. The product is dissolved in ethanol and water is added to precipitate the title compound in a yield of 0.38 g (70.3%), m.p.: 216°-217° C., [α]D20 =-109° (c=0.686, methanol).

後処理

  1. customis adjusted to 5° C.
  2. additionis dropped in
  3. stirringThe mixture is stirred for 1 additional hour
  4. waitAfter several hours
  5. filtrationthe precipitated product is filtered out
  6. washwashed with water
  7. customdried
  8. dissolutionThe product is dissolved in ethanol
  9. additionwater is added
  10. customto precipitate the title compound in a yield of 0.38 g (70.3%), m.p.: 216°-217° C., [α]D20 =-109° (c=0.686, methanol)

出典と根拠

ORDレコード
ord-7c8dccdb8c5a48e9a22679beb704e8de
出典データセット
uspto-grants-1988_10
特許番号
US04775675

反応ノート

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