Cyclohexanecarbonyl chloride → Cyclohexanecarboxylic acid {2-[4-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-piperazin-1-yl-]ethyl}-amide

HRID 381264

반응식

HRID 381264 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][NH2:19])[CH2:13][CH2:12]3)[C:5]=2[O:4][CH2:3][CH2:2]1.[CH:20]1([C:26](Cl)=[O:27])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1>ClCCl>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][NH:19][C:26]([CH:20]4[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]4)=[O:27])[CH2:15][CH2:16]3)[C:5]=2[O:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 75938Cyclohexanecarbonyl chlorideHCID 105876411-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine

생성물 1

HCID 9799670Cyclohexanecarboxylic acid {2-[4-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-piperazin-1-yl-]ethyl}-amide수율 88.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2-[4-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-piperazin-1-yl-]ethylamine (0.20 g, 0.76 mmol) in dichloromethane (5 mL) was treated with cyclohexanecarbonyl chloride (0.11 g, 0.76 mmol) at 0° C. under a nitrogen atmosphere. The resulting mixture was stirred overnight, during which time it came up to room temperature. The product was precipitated by the addition of hexane to yield the hydrochloride semihydrate salt of the titled compound (0.25 g, 80%) as a white solid; mp=165-166° C.; MS (+) ESI m/z=374 (M+H)+.

후처리

  1. customcame up to room temperature
  2. customThe product was precipitated by the addition of hexane

출처 및 근거

ORD 기록
ord-74316bd8a50748ecbdefea8f7c1c0a0c
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06306859B1

연결된 노트

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