Hydrochloric Acid → 2-[N-(2-Sulfoethyl)carbamoyl]-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline hydrochloride

HRID 1003535ノート

反応式

HRID 1003535 の反応式
P(C#N)(OCC)(OCC)=O.C(N(CC)CC)C.[C:18]([C:21]1[N:30]=[C:29]([NH:31][CH2:32][C:33]2[CH:38]=[CH:37][C:36]3[O:39][CH2:40][O:41][C:35]=3[CH:34]=2)[C:28]2[C:23](=[CH:24][CH:25]=[C:26]([Cl:42])[CH:27]=2)[N:22]=1)(O)=[O:19].[NH2:43][CH2:44][CH2:45][S:46]([O-:49])(=[O:48])=[O:47].[Na+].Cl>CN(C)C=O.O>[ClH:42].[S:46]([CH2:45][CH2:44][NH:43][C:18]([C:21]1[N:30]=[C:29]([NH:31][CH2:32][C:33]2[CH:38]=[CH:37][C:36]3[O:39][CH2:40][O:41][C:35]=3[CH:34]=2)[C:28]2[C:23](=[CH:24][CH:25]=[C:26]([Cl:42])[CH:27]=2)[N:22]=1)=[O:19])([OH:49])(=[O:48])=[O:47]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 187966952-Carboxy-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazolineHCID 23666486Sodium Taurate

生成物 1

HCID 187967922-[N-(2-Sulfoethyl)carbamoyl]-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline hydrochloride収率 173.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

0.60 ml (3.8 mmol) of diethyl cyanophosphate and 0.90 ml (6.4 mmol) of triethylamine were dropped, in this order, into a solution of 0.50 g (1.4 mmol) of 2-carboxy-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline and 0.28 g (1.9 mmol) of sodium 2-aminoethanesulfonate in 15 ml of dimethylformamide under cooling with ice and stirring. The obtained mixture was stirred at room temperature for several days, followed by the addition of 10 ml of 1N hydrochloric acid and water. The crystals thus precipitated were recovered by filtration, washed with water and air-dried to give 0.61 g of the title compound.

後処理

  1. temperatureunder cooling with ice
  2. stirringThe obtained mixture was stirred at room temperature for several days
  3. customThe crystals thus precipitated
  4. filtrationwere recovered by filtration
  5. washwashed with water
  6. customair-dried

出典と根拠

ORDレコード
ord-cf254ed0d8ec463e94bcfe9638fd8bc5
出典データセット
uspto-grants-2000_04
特許番号
US06046206

反応ノート

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