Dichloromethane → Imidazole-1-carboxylic acid (8-tert-butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-yl)-amide

HRID 1807644노트

반응식

HRID 1807644 반응식
[C:1]([C:5]1[N:14]=[CH:13][C:12]2[CH2:11][CH2:10][C:9]3[N:15]=[C:16]([NH2:18])[S:17][C:8]=3[C:7]=2[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH:19]1[N:23]=[CH:22][N:21]([C:24](N2C=NC=C2)=[O:25])[CH:20]=1.C(Cl)Cl>CN(C=O)C>[C:1]([C:5]1[N:14]=[CH:13][C:12]2[CH2:11][CH2:10][C:9]3[N:15]=[C:16]([NH:18][C:24]([N:21]4[CH:20]=[CH:19][N:23]=[CH:22]4)=[O:25])[S:17][C:8]=3[C:7]=2[N:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 682631,1'-CarbonyldiimidazoleHCID 580927368-tert-Butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-ylamine

생성물 1

HCID 86649527Imidazole-1-carboxylic acid (8-tert-butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-yl)-amide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
4 °C

실험 절차

8-tert-Butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-ylamine (Stage A.1, 0.319 g, 1.225 mmol) and CDI (278 mg, 1.715 mmol) were added to DCM (5 ml) and DMF (0.25 ml) under an argon atm. After 18 h the residue was cooled to 4° C. and the precipitate was collected by filtration. The solid was dried at 50° C. in high vacuo to give the title compound as a pale yellow solid. LCMS: tR 0.95 min and M+H 319.0 (method A2) for (8-tert-butyl-4,5-dihydro-thiazolo[4,5-h]quinazolin-2-yl)-carbamic acid methyl ester; the product of the reaction of the title compound with MeOH during the preparation of the sample as MeOH solution.

후처리

  1. filtrationthe precipitate was collected by filtration
  2. customThe solid was dried at 50° C. in high vacuo

출처 및 근거

ORD 기록
ord-f0060a546aca4b29adc7e2fed8c88a86
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357707B2

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