Diisopropylethylamine → HCID 178476471, 화합물

HRID 278618노트

반응식

HRID 278618 반응식
Cl.[C:2]([NH:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([C:12]([N:14]2[CH2:19][CH2:18][N:17]([S:20]([C:23]3[CH:32]=[CH:31][C:30]4[C:25](=[CH:26][CH:27]=[C:28]([Cl:33])[CH:29]=4)[CH:24]=3)(=[O:22])=[O:21])[CH2:16][CH2:15]2)=[O:13])[CH2:8][CH2:7]1)(=[NH:4])[CH3:3].[C:34]([O:37][CH:38]([O:40][C:41](C1C=C([N+]([O-])=O)C=CC=1O)=[O:42])[CH3:39])(=[O:36])[CH3:35].C(N(C(C)C)CC)(C)C>CN(C=O)C>[C:34]([O:37][CH:38]([O:40][C:41]([CH2:3][C:2]([NH:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([C:12]([N:14]2[CH2:19][CH2:18][N:17]([S:20]([C:23]3[CH:32]=[CH:31][C:30]4[C:25](=[CH:26][CH:27]=[C:28]([Cl:33])[CH:29]=4)[CH:24]=3)(=[O:22])=[O:21])[CH2:16][CH2:15]2)=[O:13])[CH2:8][CH2:7]1)=[NH:4])=[O:42])[CH3:39])(=[O:36])[CH3:35]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 23447477HCID 23447477, 화합물HCID 178465618HCID 178465618, 화합물

생성물 1

HCID 178476471HCID 178476471, 화합물수율 75.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 1-(trans-4-acetimidoylaminocyclohexane-1-ylcarbonyl)-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (100 mg), 0-(1-acetoxyethoxycarbonyl)-4-nitrophenol (63 mg) and diisopropylethylamine (72 mg) in DMF (4 ml) was stirred at 50t for 15 hours. The reaction solution was concentrated, and the residue was dissolved in ethyl acetate, washed with water, sodium hydrogen carbonate aqueous solution and brine, dried and concentrated. The residue was purified with silica gel column chromatography (ethyl acetate) to give a colorless solid of the title compound (89 mg).

후처리

  1. concentrationThe reaction solution was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water, sodium hydrogen carbonate aqueous solution and brine
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified with silica gel column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-f24fa10cb1324cc69b4d0110c5bc57e2
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359134B1

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