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

Dichloromethane → HCID 18706970、化合物

HRID 1422071
ノート
印刷プレビュー

反応式

HRID 1422071 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:16]([CH2:30][CH3:31])=[C:17]3[CH:25]=[CH:24][CH:23]=[C:22]4[N:18]3[C:19]=2[CH:20]=[C:21]4[C:26]([O:28]C)=[O:27])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].ClCCl>CO.O>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:16]([CH2:30][CH3:31])=[C:17]3[CH:25]=[CH:24][CH:23]=[C:22]4[N:18]3[C:19]=2[CH:20]=[C:21]4[C:26]([OH:28])=[O:27])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 14797Potassium HydroxideHCID 11144022HCID 11144022、化合物

生成物 1

HCID 18706970HCID 18706970、化合物収率 26.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

Methyl 3-(4-benzyloxyphenyl)-4-ethylpyrrolo[2,1,5-cd]indolizine-1-carboxylate (2.92 g, 7.13 mmol) was dissolved in 200 ml of methanol and 20 ml of water. Potassium hydroxide (6.40 g, 114 mmol) was added and the mixture was heated to reflux for 3 days. The reaction mixture was allowed to cool to room temperature and the methanol was evaporated. The orange solid was partitioned between 200 ml of dichloromethane and 200 ml of 1M hydrochloric acid and acidified with concentrated hydrochloric acid until pH=1. This resulted in the formation of a suspension. A further 800 ml of dichloromethane and 200 ml of water was added and the suspension was filtered to give 0.74 g (26%) of 3-(4-benzyloxyphenyl)-4-ethylpyrrolo[2,1,5-cd]indolizine-1-carboxylic acid as a yellow solid. The organic solution was washed with brine, dried over magnesium sulfate and evaporated to give a orange solid. This solid was recrystallised from acetone to afford 1.23 g (43%) of 3-(4-benzyloxyphenyl)-4-ethylpyrrolo[2,1,5-cd]indolizine-1-carboxylic acid as a yellow solid. M.p. 223-224° C. MS(SP): m/z 395 (M+). 1H-NMR (DMSO-d6, 200 MHz) δ: 1.41 (t, 3H); 3.02 (q, 2H); 5.22 (s, 2H); 7.24 (d, 2H); 7.31-7.56 (m, 5H); 7.81 (d, 2H); 7.95 (t, 1H); 8.03 (s, 1H); 8.20 (d, 1H); 8.32 (d, 1H); 12.46 (bs, 1H).

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 3 days
  3. customthe methanol was evaporated
  4. customThe orange solid was partitioned between 200 ml of dichloromethane and 200 ml of 1M hydrochloric acid
  5. customThis resulted in the formation of a suspension
  6. filtrationthe suspension was filtered

出典と根拠

ORDレコード
ord-71a4bf4dbba74c668deb1f9ca2e2ceed
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06080754

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート