Benzene → N-(2,2-dipropoxyethyl)-N-(4-methyl-1,3-dioxolan-2-ylmethyl)-alpha-chloroacetamide

HRID 1111562노트

반응식

HRID 1111562 반응식
[CH2:1]([O:4][CH:5]([O:15][CH2:16][CH2:17][CH3:18])[CH2:6][NH:7][CH2:8][CH:9]1[O:13][CH:12]([CH3:14])[CH2:11][O:10]1)[CH2:2][CH3:3].C1C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+].[Cl:31][CH2:32][C:33](Cl)=[O:34]>O>[CH2:16]([O:15][CH:5]([O:4][CH2:1][CH2:2][CH3:3])[CH2:6][N:7]([CH2:8][CH:9]1[O:13][CH:12]([CH3:14])[CH2:11][O:10]1)[C:33](=[O:34])[CH2:32][Cl:31])[CH2:17][CH3:18]

참가 물질

6

반응물 4

HCID 241BenzeneHCID 6577Chloroacetyl chlorideHCID 10340Sodium CarbonateHCID 22766279N-(2,2-dipropoxyethyl)-N-(4-methyl-1,3-dioxolan-2-ylmethyl)amine

생성물 1

HCID 22766285N-(2,2-dipropoxyethyl)-N-(4-methyl-1,3-dioxolan-2-ylmethyl)-alpha-chloroacetamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

N-(2,2-Dipropoxyethyl)-N-(4-methyl-1,3-dioxolan-2-ylmethyl)amine (0.05 mole), benzene (100 ml), water (100 ml) and sodium carbonate (2 grams) are charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The reaction mixture is cooled to a temperature of from 5° to 10° C and chloroacetyl chloride (0.05 mole) is added dropwise with stirring. After the addition is completed stirring is continued until the reaction mixture has reached room temperature. After this time the organic phase is separated from the aqueous phase and is washed with water. The washed solution is then dried over anhydrous magnesium sulfate, filtered and stripped of solvent under reduced pressure to yield the desired product N-(2,2-dipropoxyethyl)-N-(4-methyl-1,3-dioxolan-2-ylmethyl)-α-chloroacetamide as the residue.

후처리

  1. customequipped with a mechanical stirrer
  2. additionis added dropwise
  3. additionAfter the addition
  4. stirringis completed stirring
  5. customhas reached room temperature
  6. customAfter this time the organic phase is separated from the aqueous phase
  7. washis washed with water
  8. dry with materialThe washed solution is then dried over anhydrous magnesium sulfate
  9. filtrationfiltered

출처 및 근거

ORD 기록
ord-27b0756a666645448ce14d345f0b7e62
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04118216

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