Methyl bromoacetate → HCID 57238497, 화합물

HRID 848929노트

반응식

HRID 848929 반응식
Br.[C:2]([O:6][C:7]([CH2:9][N:10]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17][N:16]([CH2:22][C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:15][CH2:14][N:13]([CH2:30][C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:12][CH2:11]1)=[O:8])([CH3:5])([CH3:4])[CH3:3].Br[CH2:39][C:40]([O:42][CH3:43])=[O:41]>C(#N)C>[C:2]([O:6][C:7]([CH2:9][N:10]1[CH2:21][CH2:20][N:19]([CH2:39][C:40]([O:42][CH3:43])=[O:41])[CH2:18][CH2:17][N:16]([CH2:22][C:23]([O:25][C:26]([CH3:27])([CH3:28])[CH3:29])=[O:24])[CH2:15][CH2:14][N:13]([CH2:30][C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:12][CH2:11]1)=[O:8])([CH3:5])([CH3:3])[CH3:4]

참가 물질

4

반응물 2

HCID 60984Methyl bromoacetateHCID 21832608Tri-tert-butyl 2,2',2''-(1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetate--hydrogen bromide (1/1)

생성물 1

HCID 57238497HCID 57238497, 화합물수율 95%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1,4,7-Tri-tertbutoxycarbonylmethyl-1,4,7,10-tetraazacyclododecane hydrobromide (25.0 g, 42 mmol) was slurried in acetonitrile and treated with TMG (70 mL). Methyl bromoacetate (6.5 g, 42 mmol) was added in one portion, and the mixture was refluxed for 3 hours. After stirring at ambient temperature for an additional 18 hours, the solvent and excess TMG were removed by rotary evaporation. The residue was dissolved in CHCl3, washed with water, and dried (Na2SO4). Evaporation of the solvent afforded the title product as a pale oil (23 g, 95%). 1H NMR (CDCl3): 1.4 (s, 27 H) , 2.8 (s, 16 H), 3.2 (s, 6 H), 3.4 (s 2 H), 3.6 (s, 3 H).

후처리

  1. additiontreated with TMG (70 mL)
  2. temperaturethe mixture was refluxed for 3 hours
  3. customthe solvent and excess TMG were removed by rotary evaporation
  4. dissolutionThe residue was dissolved in CHCl3
  5. washwashed with water
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-fa29adbdc0ae47d1b2f9483f8aaf1629
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06010681

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