ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1,2-Dichloroethane → HCID 86758351、化合物

HRID 2229221
ノート
印刷プレビュー

反応式

HRID 2229221 の反応式
[CH2:1]([O:3][P:4]([C:9]1[C:10](=[O:21])[NH:11][C:12]2[C:17]([CH:18]=1)=[CH:16][C:15]([NH2:19])=[C:14]([Cl:20])[CH:13]=2)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].CO[CH:24]1[CH2:28][CH2:27][CH:26](OC)O1.C(O)(=O)C.ClCCCl>O.C(Cl)Cl.CO>[CH2:1]([O:3][P:4]([C:9]1[C:10](=[O:21])[NH:11][C:12]2[C:17]([CH:18]=1)=[CH:16][C:15]([N:19]1[CH:24]=[CH:28][CH:27]=[CH:26]1)=[C:14]([Cl:20])[CH:13]=2)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 176Acetic AcidHCID 790982,5-Dimethoxytetrahydrofuran2 回HCID 15511753HCID 15511753、化合物

生成物 1

HCID 86758351HCID 86758351、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 21226129
Dichloromethane methanol
溶媒

反応条件

温度
75 °C

実験手順

A biphasic suspension of 2.43 g (7.35 mmol) of the compound obtained in Step D of Example 1 and 1.33 ml (10.29 mmol) of 2,5-dimethoxytetrahydrofuran in a mixture of 24 ml of distilled water, 12 ml of acetic acid and 36 ml of 1,2-dichloroethane is stirred vigorously at 75° C. for 60 minutes. In TLC (CH2Cl2/MeOH 9:1), a small amount of starting material is still observed. 0.2 eq. of 2,5-dimethoxytetrahydrofuran (2.06 mmol, 0.26 ml) is added, and heating is maintained for 30 minutes. The mixture is left to return to room temperature and extraction is carried out with CH2Cl2. The organic phase is washed 4 times with water and then with a saturated NaCl solution. Drying is carried out over MgSO4, followed by evaporation and chromatography of the resulting oil over 200 g of Merck 7734 silica whilst eluting with a mixture of CH2Cl2/MeOH 95:5. An oil corresponding to the title product is obtained, which is crystallised from isopropyl ether.

後処理

  1. temperatureheating
  2. temperatureis maintained for 30 minutes
  3. waitThe mixture is left
  4. customto return to room temperature
  5. extractionextraction
  6. washThe organic phase is washed 4 times with water
  7. customDrying
  8. customfollowed by evaporation and chromatography of the resulting oil over 200 g of Merck 7734 silica
  9. washwhilst eluting with a mixture of CH2Cl2/MeOH 95:5

出典と根拠

ORDレコード
ord-110df0efd9fd49ad8c8f6841ba6f8c03
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06420386B1

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート