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Triethylamine → HCID 131711060, 화합물

HRID 1679624
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HRID 1679624 반응식
C(N(CC)CC)C.[NH2:8][CH:9]1[C:19](=[O:20])[N:11]2[CH:12]([C:17]#[N:18])[C:13]([CH3:16])([CH3:15])[S:14][C@H:10]12.[CH3:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:28](Cl)([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[CH3:41])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>C(Cl)Cl>[CH3:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:28]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[CH3:41])([NH:8][CH:9]1[C:19](=[O:20])[N:11]2[CH:12]([C:17]#[N:18])[C:13]([CH3:15])([CH3:16])[S:14][C@H:10]12)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 22750484HCID 22750484, 화합물HCID 70604619HCID 70604619, 화합물

생성물 1

HCID 131711060HCID 131711060, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
-10 °C

실험 절차

Triethylamine (444 mg., 4.4 mmole) is added to a suspension of 6-amino-2,2-dimethyl-3-cyanopenam (468 mg., 2 mmole) in methylene chloride (20 ml.) and the resulting mixture cooled to -10° C. A solution of α,α-di(2-methylphenyl) benzyl chloride (614 mg., 2 mmole) in methylene chloride (12 ml.) is added over a ten minute period and the resulting yellow solution stirred for 1 hour at -10° C. The cooling bath is removed and the mixture stirred and allowed to warm to room temperature. It is stirred for two hours at room temperature and is then concentrated under reduced pressure to a brown sludge. The sludge is chromatographed on a silica gel column (70-23- mesh., 380 × 20 mm. column) using chloroform as eluent. Fractions (15 ml. each) are collected. Fractions 13-19 are combined and concentrated in vacuo to dryness to give 155 mg. of product as a foam.

후처리

  1. customThe cooling bath is removed
  2. stirringthe mixture stirred
  3. temperatureto warm to room temperature
  4. stirringIt is stirred for two hours at room temperature
  5. concentrationis then concentrated under reduced pressure to a brown sludge
  6. customThe sludge is chromatographed on a silica gel column (70-23- mesh., 380 × 20 mm. column)
  7. customeach) are collected
  8. concentrationconcentrated in vacuo to dryness
  9. customto give 155 mg

출처 및 근거

ORD 기록
ord-8e4091961341462b835ea158deab2bb7
출처 데이터셋
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04081455

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