Water → HCID 18365419, 화합물

HRID 380638노트

반응식

HRID 380638 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-4708adf9e56e4145ad92043dc65d8717
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303633B1

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