Phosphoric Acid → HCID 23649026、化合物

HRID 1676902ノート

反応式

HRID 1676902 の反応式
[OH:1][P:2]([OH:5])([OH:4])=[O:3].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[NH2:20][C:21]1([CH2:40]O)[CH2:25][CH2:24][CH:23]([C:26]2[CH:31]=[CH:30][C:29]([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])=[CH:28][CH:27]=2)[CH2:22]1>O>[P:2]([OH:5])([OH:4])([O:1][CH2:40][C:21]1([NH2:20])[CH2:25][CH2:24][CH:23]([C:26]2[CH:27]=[CH:28][C:29]([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])=[CH:30][CH:31]=2)[CH2:22]1)=[O:3]

参加物

5

反応物 3

HCID 1004Phosphoric AcidHCID 14812Phosphorus oxide (P4O10)2 回HCID 11623636HCID 11623636、化合物

生成物 1

HCID 23649026HCID 23649026、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

1 mL of 85% H3PO4 was slowly added (by drops) into 0.5 g of P2O5, the acid-anhydride mixture was then heated at 100° C. for 1 hour under nitrogen protection. Another 0.5 g of P2O5 and 30 mg of alcohol 6 were added to the poly phosphoric acid and heated for 5 hours at 100° C. After cooling down to room temperature, 10 mL cold water (0° C.) was added to reaction mixture. The product precipitated out as white solid, was collected and washed with water. 31 mg (82%) of green colored product was collected after vacuum drying. MS only two peaks: M+1=384.4 with 304.4 (hydrolyzed back to 6).

後処理

  1. temperatureAfter cooling down to room temperature
  2. customThe product precipitated out as white solid
  3. customwas collected
  4. washwashed with water
  5. custom31 mg (82%) of green colored product was collected after vacuum
  6. customdrying

出典と根拠

ORDレコード
ord-746b874dec4d4c0db55c03dca97a610f
出典データセット
uspto-grants-2011_08
特許番号
US08008286B2

反応ノート

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