Water → HCID 18365419, 화합물

HRID 1899874노트

반응식

HRID 1899874 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 18365419HCID 18365419, 화합물수율 100%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-347043f1fa4f4e92b98ba17f59620c51
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05574046

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