Ethyl 4-chlorobutyrate → 3-Acetyl-2-[2-[3-(ethoxycarbonyl)-propoxy]phenyl]benzothiazoline

HRID 637754

반응식

HRID 637754 반응식
[H-].[Na+].[C:3]([N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[S:8][CH:7]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[OH:21])(=[O:5])[CH3:4].Cl[CH2:23][CH2:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27]>CN(C=O)C>[C:3]([N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[S:8][CH:7]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[O:21][CH2:23][CH2:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])(=[O:5])[CH3:4]

참가 물질

5

반응물 3

HCID 18474Ethyl 4-chlorobutyrateHCID 24758Sodium hydrideHCID 133359603-Acetyl-2-(2-hydroxyphenyl)benzothiazoline

생성물 1

HCID 135642173-Acetyl-2-[2-[3-(ethoxycarbonyl)-propoxy]phenyl]benzothiazoline

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

To the suspension of 1.59 g of sodium hydride in 30 ml of anhydrous DMF, the solution of 8.13 g of 3-acetyl-2-(2-hydroxyphenyl)benzothiazoline in 30 ml of anhydrous DMF is added dropwise under nitrogen atmosphere at room temperature. After the addition, the reaction mixture is stirred for 20 minutes at room temperature. To the reaction mixture, the solution of 4.95 g of ethyl 4-chlorobutyrate in 15 ml of anhydrous DMF is added and stirred for 5 hours at 70° C. After cooling to room temperature the reaction mixture is poured into ice-water and extracted with ethyl acetate.

후처리

  1. additionAfter the addition
  2. stirringstirred for 5 hours at 70° C
  3. temperatureAfter cooling to room temperature the reaction mixture
  4. extractionextracted with ethyl acetate

출처 및 근거

ORD 기록
ord-172096d1e1094eb0acee96098768111b
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558125

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