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

HRID 1807644ノート

反応式

HRID 1807644 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
4 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f0060a546aca4b29adc7e2fed8c88a86
出典データセット
uspto-grants-2013_01
特許番号
US08357707B2

反応ノート

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