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Triethylamine → HCID 15614750, 화합물

HRID 1084528
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HRID 1084528 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[O:19])[CH:10]([CH2:20][NH2:21])[N:9]=1.[NH:22]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:24]=[C:23]1[C:31](Cl)=[O:32].C(N(CC)CC)C>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[O:19])[CH:10]([CH2:20][NH:21][C:31]([C:23]2[NH:22][C:30]3[C:25]([CH:24]=2)=[CH:26][CH:27]=[CH:28][CH:29]=3)=[O:32])[N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 118162081H-indole-2-carbonyl ChlorideHCID 15614835HCID 15614835, 화합물

생성물 1

HCID 15614750HCID 15614750, 화합물수율 32.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,3-Dihydro-5-(2-fluorophenyl)-3(RS)-aminomethyl-2H-1,4-benzodiazepin-2-one (80 mg, 0.282 mmole) and indole-2-carbonyl chloride (53 mg, 0.30 mmol) were mixed in 5 ml of methylene chloride at room temperature. The homogeneous reaction mixture was protected from moisture and treated with 42 l (0.30 mmole) of triethylamine. Within five min., triethylamine hydrochloride precipitated. The reaction mixture was stirred at room temperature overnight and then partitioned between methylene chloride and saturated sodium bicarbonate solution. The resulting solid was collected, washed with water and dried over P2O5 at 70° C. In this way, 39 mg of the analytical product was obtained, m.p.: 315°-317° (d).

후처리

  1. customtriethylamine hydrochloride precipitated
  2. custompartitioned between methylene chloride and saturated sodium bicarbonate solution
  3. customThe resulting solid was collected
  4. washwashed with water
  5. dry with materialdried over P2O5 at 70° C

출처 및 근거

ORD 기록
ord-5f92fc1c6952408ebd6031c1e3f5e911
출처 데이터셋
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05004741

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