Water → HCID 18365419、化合物

HRID 1899874ノート

反応式

HRID 1899874 の反応式
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([C:11](=[O:27])[CH2:12][CH2:13][CH:14]3[CH2:19][CH2:18][N:17]([CH2:20]C4C=CC=CC=4)[CH2:16][CH2:15]3)[CH:8]=[CH:7][C:5]=2[N:6]=1.ClC(O[CH:32]([Cl:34])[CH3:33])=O.[OH2:35]>ClCCCl>[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([C:11](=[O:27])[CH2:12][CH2:13][CH:14]3[CH2:19][CH2:18][N:17]([C:20]([CH:32]([Cl:34])[CH3:33])=[O:35])[CH2:16][CH2:15]3)[CH:8]=[CH:7][C:5]=2[N:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 192442245365-80-4HCID 5213051-Chloroethyl chloroformate

生成物 1

HCID 18365419HCID 18365419、化合物収率 100%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 0.90 g (2.38 mM) of 1-(2-methyl-6-benzthiazolyl)-3-[1-(phenylmethyl)-4-piperidinyl]-1-propanone (Example 27) and 0.33 mL (3.1 mM) of 1-chloroethyl chloroformate was refluxed in 10 mL of 1,2-dichloroethane for 2 hours. The resulting brown solution was cooled to room temperature and diluted with 15 mL of water. This mixture was extracted twice with 20 mL of ethyl acetate. The ethyl acetate extracts were combined, dried (Na2SO4), and evaporated to yield 1.0 g (100%) 1-(2-methyl-6-benzothiazolyl)-3-[(1-chloroethylformyl)-4-piperidinyl]-1-propanone as an oil.

後処理

  1. extractionThis mixture was extracted twice with 20 mL of ethyl acetate
  2. dry with materialdried (Na2SO4)
  3. customevaporated

出典と根拠

ORDレコード
ord-347043f1fa4f4e92b98ba17f59620c51
出典データセット
uspto-grants-1996_11
特許番号
US05574046

反応ノート

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