Di-p-tolylcarbodiimide → HCID 178426524, 화합물

HRID 1813887노트

반응식

HRID 1813887 반응식
Cl.[CH2:2]([O:9][C:10](=[O:23])[C@H:11]([CH2:13][C:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[NH:16][CH:15]=1)N)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([N:27](C(C)C)CC)(C)C.[C:33]1([CH3:49])[CH:38]=[CH:37][C:36]([N:39]=[C:40]=[N:41][C:42]2[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][CH:43]=2)=[CH:35][CH:34]=1>CN(C=O)C>[C:33]1([CH3:49])[CH:38]=[CH:37][C:36]([N:39]([CH:11]([CH2:13][C:14]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[NH:16][CH:15]=2)[C:10]([O:9][CH2:2][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)=[O:23])[C:40]([NH:41][C:42]2[CH:43]=[CH:44][C:45]([CH3:48])=[CH:46][CH:47]=2)=[NH:27])=[CH:35][CH:34]=1

참가 물질

5

반응물 3

HCID 69763Di-p-tolylcarbodiimideHCID 81531DiisopropylethylamineHCID 45073232L-tryptophan benzyl ester hydrochloride

생성물 1

HCID 178426524HCID 178426524, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.0 mmol of tryptophan benzyl ester hydrochloride was dissolved in 20 ml of DMF and 1.1 mmol of diisopropylethylamine was added. After 10 min, 1.0 mmol of 1,3 di-p-tolylcarbodiimide was added to the stirred solution. The reaction mixture was stirred overnight in room temperature. The precipitated solid was filtered off and washed twice with 1 ml of DMF. To the collected filtrate, 50 ml of water was added. The precipitated solid was collected by filtration and washed with water. The solid was dissolved in ethyl acetate and 0.1 ml of conc. HCl was added. The pure product was precipitated from the solution with ethyl ether. Yield of pure compound=79%.

후처리

  1. filtrationThe precipitated solid was filtered off
  2. washwashed twice with 1 ml of DMF
  3. additionTo the collected filtrate, 50 ml of water was added
  4. filtrationThe precipitated solid was collected by filtration
  5. washwashed with water
  6. dissolutionThe solid was dissolved in ethyl acetate
  7. addition0.1 ml of conc. HCl was added
  8. customThe pure product was precipitated from the solution with ethyl ether

출처 및 근거

ORD 기록
ord-f3d466c8f3b941adb6358af8846a5256
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06875759B1

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