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Chloroacetyl chloride → HCID 18946297, 화합물

HRID 1768948
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HRID 1768948 반응식
[N:1]1([C:6]2[N:11]=[C:10]([N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[CH:9]=[C:8]([N:18]3[CH2:22][CH2:21][CH2:20][CH2:19]3)[N:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:23][CH2:24][C:25](Cl)=[O:26]>C(Cl)(Cl)Cl>[Cl:23][CH2:24][C:25]([N:15]1[CH2:16][CH2:17][N:12]([C:10]2[CH:9]=[C:8]([N:18]3[CH2:19][CH2:20][CH2:21][CH2:22]3)[N:7]=[C:6]([N:1]3[CH2:5][CH2:4][CH2:3][CH2:2]3)[N:11]=2)[CH2:13][CH2:14]1)=[O:26]
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참가 물질

4

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HCID 6577Chloroacetyl chlorideHCID 145852434-(Piperazin-1-yl)-2,6-di(pyrrolidin-1-yl)pyrimidine

생성물 1

HCID 18946297HCID 18946297, 화합물수율 97%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

The starting 1-(2-chloroacetyl)-4-[2,6-di(1-pyrrolidinyl)-4-pyrimidinyl]piperazine was prepared as follows: 1-[2,6-di(1-pyrrolidinyl)-4-pyrimidinyl]piperazine (1.65 g, 5.4 mmol) was dissolved in anhydrous chloroform (30 ml), the solution was cooled to 0°-5° C. and 2-chloroacetyl chloride (0.50 ml, 0.79 g, 7.0 mmol) in anhydrous chloroform (5 ml) was added dropwise under stirring. The mixture was stirred for one hour, concentrated and the residue was dissolved in 100 ml of water. The aqueous solution was made alkaline with conc. NH4OH and stirred for one hour. During this period the separated oil solidified. The solids were collected, washed with icecold water until neutral and dried. In this manner 2.0 g of the desired chloroacetyl compound was obtained, yield: 97.0% mp. 153°-156° C.

후처리

  1. temperaturethe solution was cooled to 0°-5° C.
  2. stirringThe mixture was stirred for one hour
  3. concentrationconcentrated
  4. dissolutionthe residue was dissolved in 100 ml of water
  5. stirringstirred for one hour
  6. waitDuring this period the separated oil solidified
  7. customThe solids were collected
  8. washwashed with icecold water until neutral and
  9. customdried

출처 및 근거

ORD 기록
ord-8999d8a487e242dcafe8d4189c64edc7
출처 데이터셋
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05380724

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