Triethylamine → HCID 178453908, 화합물

HRID 645462

반응식

HRID 645462 반응식
Cl.[CH2:2]1[C:10]2[C:5](=[C:6]([N:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.[C:17]([O:21][C:22](=[O:33])[NH:23][C@H:24]1[CH2:29][CH2:28][C@H:27]([CH2:30][CH:31]=O)[CH2:26][CH2:25]1)([CH3:20])([CH3:19])[CH3:18].C(N(CC)CC)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])[O-].[K+].[K+]>ClC(Cl)C.O>[C:17]([O:21][C:22](=[O:33])[NH:23][C@H:24]1[CH2:25][CH2:26][C@H:27]([CH2:30][CH2:31][N:14]2[CH2:13][CH2:12][N:11]([C:6]3[CH:7]=[CH:8][CH:9]=[C:10]4[C:5]=3[CH2:4][CH2:3][CH2:2]4)[CH2:16][CH2:15]2)[CH2:28][CH2:29]1)([CH3:20])([CH3:19])[CH3:18]

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 210731941-Indan-4-yl-piperazine hydrochlorideHCID 178453924HCID 178453924, 화합물

생성물 1

HCID 178453908HCID 178453908, 화합물수율 85.8%

시약·촉매·용매 2

HCID 962Water용매HCID 63651,1-Dichloroethane용매

실험 절차

3.58 g (15 mmol) of 1-(indan-4-yl)-piperazine hydrochloride and 3.62 g (15 mmol) of trans-4-(2-oxoethyl)cyclohexyl-carbamic acid tert-butyl ester were dissolved in dichloroethane (120 ml), 2.1 ml (15 mmol) triethylamine was added, then 4.6 g (22 mmol) sodium triacetoxyborohydride was added portionswise and the reaction mixture was stirred for 20 hours at ambient temperature, then 20% potassium carbonate solution in water (40 ml) was added. The organic layer was separated, dried and evaporated to dryness in vacuo. The precipitate was recrystallized from acetonitrile to give the title compound 5.5 g (yield: 85.8%), m.p.: 115-8° C.

후처리

  1. customThe organic layer was separated
  2. customdried
  3. customevaporated to dryness in vacuo
  4. customThe precipitate was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-ad46cd87e58e41deb98dd2372c7fa4f6
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07705003B2

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