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Sulfuric Acid → HCID 10815838, 화합물

HRID 1034027
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HRID 1034027 반응식
[CH2:1]([O:3][C:4]1[CH:14]=[C:13]([CH2:15][C:16]#[N:17])[CH:12]=[CH:11][C:5]=1[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].[CH:18]1([CH2:24][CH:25](O)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[N:32]2[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.S(=O)(=O)(O)[OH:40]>ClC1C=CC=CC=1Cl>[CH2:1]([O:3][C:4]1[CH:14]=[C:13]([CH2:15][C:16]([NH:17][CH:25]([CH2:24][CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[N:32]2[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]2)=[O:40])[CH:12]=[CH:11][C:5]=1[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 10489807Benzoic acid, 4-(cyanomethyl)-2-ethoxy-, ethyl esterHCID 54424526HCID 54424526, 화합물

생성물 1

HCID 10815838HCID 10815838, 화합물

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매2회

실험 절차

At 23°-25° C., a solution of ethyl 2-ethoxy-4-cyanomethyl-benzoate (2.35 g, 10 mmol) and α-cyclohexylmethyl-2-piperidino-benzyl alcohol (2.88 g, 10 mmol) in o-dichlorobenzene (15 ml) is added dropwise to a mixture of concentrated sulphuric acid (15 ml) and o-dichlorobenzene (15 ml). The mixture is stirred for 2 hours at ambient temperature. The o-dichlorobenzene phase is then separated off and the residue is added to ice. After being made alkaline with soda solution, it is extracted with chloroform. The extracts are dried over sodium sulphate and concentrated by evaporation. The residue is purified by column chromatography on silica gel (toluene/acetone=10/1). Yield: 1.1 g

후처리

  1. customThe o-dichlorobenzene phase is then separated off
  2. additionthe residue is added to ice
  3. extractionis extracted with chloroform
  4. dry with materialThe extracts are dried over sodium sulphate
  5. concentrationconcentrated by evaporation
  6. customThe residue is purified by column chromatography on silica gel (toluene/acetone=10/1)

출처 및 근거

ORD 기록
ord-b3db1fb1df8049ae8945955ee860882c
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05312924

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